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By R. A. Wood, R. I. Jaffee, H. R. Ogden, D. N. Williams

The tensile properties, creep resistance. and thermal stability of highly alloyed Ti-Al-Zr alloys were examined. On the basis of these studies, the Ti-7Al-1ZZr composition was selected for more complete evaluation. The alloy was found to be weldable and free from excessive directionality. In addition, it developed maximum properties without requiring heat treatment other than an annealing operation in the alpha field. The alloy was recommended for scale up and is presently being investigated on a production-level basis. One of the more attractive properties of titanium alloys is their ability to withstand stress at moderately high temperatures, and a considerable amount of effort has been devoted to increasing the maximum service temperature of titanium alloys. This work has suggested that the optimum alloys for high-temperature service will be single-phase a (close-packed hexagonal) alloys containing significant amounts of aluminum. However, the maximum amount of aluminum which can be alloyed with titanium is between 6 and 8 pct,l since at high-aluminum contents an embrittlement reaction occurs in the anticipated service temperature range, 800" to 1100°F. It has been shown that the embrittlement reaction involves decomposition of the high-aluminum a phase to one or more new phases.' Since this reaction does not occur at intermediate or low-aluminum contents, it was felt that intermediate Ti-A1 alloys might be strengthened by a-soluble ternary additions without inducing the embrittlement reaction. The first alloying addition considered was tin, which shows extensive solubility in a titanium and has moderate strengthening tendencies. Unfortunately, it was soon apparent that tin also promoted the embrittlement reaction, and that to obtain a stable alloy, the aluminum content had to be reduced as the tin content was increased. The second alloying addition considered was zirconium, which is similar to tin in its effects on titanium. This element did not contribute to the embrittlement reaction and, in fact, appeared to increase the maximum amount of aluminum which could be alloyed with titanium without inducing instability. This paper describes an investigation of the Ti-A1-Zr a alloy region. Alloys containing from 4 to 12 pct A1 and from 6 to 15 pct Zr were examined. The properties of these alloys are described and the bases for selecting an optimum composition is outlined. This composition, Ti-7A1-12Zr, is presently being scaled up in tonnage quantities, and is being evaluated extensively throughout the industry. In addition to presenting the basis for its selection, this paper presents a description of the properties developed in laboratory material as determined during the alloy investigation. These properties suggest that this alloy can fill an important position in applications requiring light weight, fabrica-bility, weldability, and strength to 1000oF or higher. EXPERIMENTAL PROCEDURES Titanium alloy ingots were prepared by inert electrode arc melting under an argon atmosphere. Alloying elements used were 110 Bhn titanium sponge, high-purity aluminum, and reactor-grade zirconium. Pancake-shaped ingots were prepared weighing approximately 300 g. The composition of the ingots was checked by weight measurements before and after melting. The pancake ingots were forged at 2000°F to approximately half their original thickness to give a flat plate roughly 1/2 in. thick. This plate was then rolled at 1800' to 1600°F to 0.250 in. thick. All of the alloys examined fabricated well. However, alloys containing 15 pct Zr tended to overheat due to exothermic oxidation, and scaling was excessive. As might be anticipated from its effect in decreasing the ß transus, increased zirconium appeared to improve fabricability somewhat, especially during rolling at lower temperatures. Except for a limited study of heat-treatment response, all alloys were examined in the a-annealed condition. Prior to heat treatment the a and ß tran-sus temperatures were determined by metallo-graphic examination of samples quenched after annealing at 50-deg intervals in the transformation region. These data are shown in Fig. 1. Recrystal-lization appeared to occur in about 1 hr in the range 1300º to 1500ºF. Therefore, alloys were annealed for 1 hr at 1550ºF (4 and 5 pct Al), 1600ºF (6 through 7-1/2 pct Al), or 1650°F (8 or more pct Al). This produced an equiaxed a grain structure. In most alloys, a "ghost" structure was visible after the a-annealing treatment, as shown in Fig. 2. This structure apparently resulted from the acicular

Jan 1, 1963

By C. H. Gorski

A method for preparing titanium tetrachloride is described which consists of reducing rutile with coke and chlorinating the reduced product at 200° to 500°C. The crude distillate is purified by treatment with copper powder and distillation. Recoveries, exceeding 90 pct of the titanium in the rutile, were obtained. IN recent years considerable interest in metallic titanium has been aroused because of its outstanding physical and chemical properties. The present commercial processes for preparing titanium are modifications of the Kroll1 process and consist essentially of the reduction of titanium tetrachloride with magnesium in an inert atmosphere to produce metallic titanium with magnesium chloride as a byproduct. At present,' commercial titanium tetrachloride costs $0.32 a pound, which makes the price of the included titanium $1.28 a pound. As the titanium tetrachloride must be purified further before processing into metal, its ultimate cost obviously will be higher. Consequently, one of the prime requisites for the production of lower cost titanium metal is a source of low-cost titanium tetrachloride. Recently, Knickerbocker, Gorski, Kenworthy, and Starliper3 escribed a method for preparing titanium tetrachloride from low-grade Arkansas rutile by smelting the rutile with pyrite and coke to form a titanium matte and then chlorinating the titanium matte to prepare a crude titanium tetrachloride. This process had several inherent advantages. Low-grade rutile concentrates were utilized, the chlorination temperature was relatively low (approximately 200°C), and the reaction was strongly exothermic. However, this process had several disadvantages, chief of them being the rather low recoveries of titanium tetrachloride (65 to 81 pct) and the difficulty in purifying the crude titanium tetrachloride obtained. Because of the high-titanium and low-iron con- tents of rutile as compared to ilmenite, rutile should be of greater potential value as a source of titanium tetrachloride than ilmenite. Rutile, however, is not chlorinated directly in commercial practice, because reaction temperatures above 700 °C are required, at which point chlorine attacks most of the common materials of construction. The process now in use consists of converting the titanium in rutile to the cyanonitride by high-temperature reduction in an electric furnace, and then chlorinating this compound. The disadvantages of this process are the difficulty of producing the cyanonitride, the use of high-grade rutile concentrates in the charge, and the presence of several percent of silicon tetrachloride in the finished product. It would be of considerable interest to develop a new process for the preparation of titanium tetrachloride from rutile by chlorination at 200" to 500°C. Process Development Several investigators'-' have studied the reduction of titanium dioxide with carbon in an effort to prepare titanium monoxide. Invariably, the titanium monoxide formed in this manner was not pure, as it contained titanium carbide and one or more of the lower oxides of titanium. As these lower oxides of titanium are more reactive chemically than rutile, and as it is known that titanium carbide may be chlorinated readily, a study was made of the chlorination of carbon-reduced rutile. A sample of rutile concentrates from Hot Spring County, Ark., containing 76.19 pct TiO,, 5.65 pct Fe2O3, 4.18 pct SiO2, and 2.88 pct Al2O3, was used for this investigation. The experimental procedure consisted of making an intimate mixture of —100-mesh rutile and petroleum coke, adding water and molasses as a binder to foi-m a paste, charging into a graphite crucible that was covered, except for a vent to allow the

Jan 1, 1952

By Fred B. Ely

The first recorded production in the Dutch East Indies was in the year 1893 but seepages of dl were known to exist in North Sumatra, East Java and the east coast of Borneo at least as early as 1880. During the Of the above amount the Royal Dutch produced............................................. 36,006,079 Nederlandsche Koloniale Petroleum Maatschappij (subsidiary of Standard Oil of New Jersey)....................................... 3,867,769 Total Dutch East Indiea....................................... 39,873,848

Jan 1, 1931

E. A. H. Tays, San Blas, Sinaloa, Mex. (communication to the Secretary*):—The results obtained by Messrs. Hofman and Hayward in their experiments, proving that a low percentage of copper sulphate with a variable percentage of salt, depending on the ore, gives the best results, confirm practical mill-work which I did in 1895. I have none of my notes, taken at the time, to refer to, so have to rely solely on memory, which precludes the conciseness that is alway desirable. In 1894 I took charge of the plant of the San Rafael Company, near Chinipas, Chihuahua, Mex., which at that time was treating a very refractory ore carrying about $15 in gold and from 20 to 25 oz. of silver per ton, the bullion being about 300 fine in gold. The silver in the ore was in the form of a sulphide. Although carrying an average of 0.75 oz. of gold per ton, free gold could rarely be seen by panning, but upon roasting a sample of the ore the gold became visible at once—a result which was discovered by chance and used to advantage later. In order to utilize the old mill to the best advantage, it was decided to use pan-amalgamation after roasting. The roasting, done in a lime-kiln, was similar to the ordinary " burning " operation. The roasted ore was trammed to the mill-bins and crushed by 10 stamps to pass a 30-mesh screen. The pulp was de-watered and fed to four 1-ton pans. My recollection is that upon starting the mill-work, the charge contained 1.5 lb. of copper sulphate and 5 per cent. of salt per ton. From the start the extraction was unsatisfactory and the loss of quicksilver was very large. Experiments were then carried out on a working scale. First, the quantity of copper sulphate was increased 4 oz. at a time; then it was reduced

Jan 1, 1910

By Pradeep K. Rohatgi, Clyde M. Adams

Structures produced upon solidification of the eu-tectic composition (33 wt pct Cu) aluminum copper alloy have been examined as a function of freezing rate dfs /d? , the rate of change of fraction solid (fs) with time (8). Slow (dfs/d? = 0.0016 sec-1), intermediate (dfs/d? = 0.02 sec-1) and rapid (dfs/d? = 0.4 to 7.30 sec-1) freezing rates were used. The lamellar Al-Cual2 eutectic is arranged in the form of rod-shaped colonies at rapid freezing rates. The colonies are aligned parallel to the direction of heat flow, whereas the lamellae within the colonies are aligned at various angles, as high as 90 deg, to the direction of heat flow. The colony spacing (C) is proportional to the square root of inverse freezihg rate. The relationship is C = 15.5(dfs/d?)-1/2 where C is in µ and 8 is in sec. The ratio of colony spacing to lamellar spacing is greater than 20.0 and increases with a decrease in the freezing rate. A duplex dendritic structure is produced at intermediate freezing rates. A fine lamellar eutectic is arranged within the dendrites (exhibiting side branches at an angle close to 60 deg from the main stem) and a coarse irregular eutectic appears in the interdendritic regions. The duplex eutectic structure is also produced at slow freezing rates. However, at slow freezing rates there is a Platelat of CuAl2, along the center of the main stem of each dendrite and the other lamellae are arranged perpendicular to the central platelet. THE eutectic between CuA12 and a! aluminum has been reported to freeze in a lamellar form by several workers.'-3 chadwick4 has measured the interlamel-lar spacing as a function of growth rate. Kraft and Albright2 have reported on irregularities in the lamellar structures, and have proposed growth models which account for the formation of faults during solidification. In certain instances the lamellar eutectic has been found to exist in colonies. The colony formation315 has been attributed to the breakdown of a planar liquid-solid interface due to rejection of impurities. The aim of the present work is to study the structures produced from the eutectic aluminum-copper alloy under relatively fast solidification rates, such as encountered in casting and welding operations. The solid-liquid interface presumably remains planar under conditions of slow unidirectional freezing which produce lamellae aligned parallel to the direction of heat flow. The local growth velocities are the same over the entire interface and are equal to the rate of growth of the all-solid region. The spacing between the eutectic lamellae is inversely proportional to the square root of the growth rate of the all-solid region. Under the freezing conditions used in the present study, the solid-liquid interface is cellular or dendritic and the local growth velocities are different in the different regions of the interface. The relationship between the growth rate of the all solid region and the local growth velocities varies with the location and the shape of the interface. The growth rate of the all-solid region is, therefore, an inadequate parameter to describe the eutectic micro-structures which depend upon the local growth velocities. For this reason the structures have been examined as a function of freezing rate, dfs/d?, where fs is the fraction solidified at time 0. The freezing rate was varied by a factor of 4000. The relationship between the freezing rate, dfs/d?, and the growth velocit of the all solid region depends upon the specimen geometry and the shape of the interface. EXPERIMENTAL PROCEDURES The A1-33 pct Cu alloy used throughout this study was made in an induction furnace, using electrolytic copper and aluminum of commercial purity (99.7 pct), the primary impurities being silicon (0.12 pct), iron (0.14 pct), and zinc (0.02 pct). Three ranges of freezing rates were investigated: 1) A spectrum of rapid freezing rates (ranging from 0.40 to 7.30 sec-1) was obtained in arc deposits made on 2-in. thick cast plates of the eutectic alloy. The arc was operated at constant power and was made to travel at constant velocity on the surface of the plate that was in contact with the chill surface during solidification. The pool of liquid metal formed under the moving tungsten arc solidified rapidly by heat extraction through the unmelted plate. Conditions of unidirectional heat flow were achieved near the fusion zone interface, especially in the center of the arc deposits. The great advantage of the arc technique is that rapid cooling and freezing rates can be varied in a qualitative way. The correlation between the arc parameters and the solidification rate is given by the following relationship:6-8

Jan 1, 1970

By Blamey Stevens

(San Francisco Meeting, October, 1911.) IN this paper, which is a logical extension of my paper, The Laws of Intrusion, 1 the various pressures of emanation and their mechanical causes and effects on the large scale of nature are determined, .and a classification of emanations is deduced therefrom. The Subterranean Sea. The subterranean sea is here defined as the intercommunicating water contained in the trains of pores and fissures of the rocks down to great depths. Whether the actual amount of water constituting this subterranean sea be large or small, does not enter into the present argument, since the static pressure of this water at any particular depth is not a function of the quantity : it involves only the depth and the density of the water. Densities. The total pressure at depths down to 10 or 15 miles is made up of the rock-stresses investigated in my previous papers, and the pressure of the subterranean sea. The latter component must evidently be equal to the weight of a solid column of the overlying water of unit sectional area. As water expands with heat, it should really be necessary to sum the density at every level. A knowledge of the densities of water under a variety of conditions is therefore needed, but does not seem ever to have been ascertained for such combined pressures and temperatures as we have to consider. The specific gravity of water at 28° C. for various pressures up to 400 atmospheres, has been determined by Barus,2 who

Apr 1, 1912

By L. H. Wolfe, J. O. Thieme

The tensile and shear strengths of frozen soil and the compressive strengths of ice and frozen soil were measured These tests showed that the strength of ice and of frozen soil increased as the temperature was decreased. A method is presented for the measurement of thermal conductivity and specific heat of earth and ice. Using the parameters thermal conductivity, specific heat and density, the thermal diffusivity was calculated. Results of thermal property tests establish water as the major variable contributing to thermal property values. INTRODUCTION During the last few years, a considerable interest has developed in underground storage of cryogenic liquids such as liquid natural gas. Because of its economy and safety, underground storage is being used. Before underground caverns could be seriously considered, however, the strength and thermal characteristics of the soil had to be obtained. Methods are presented herein for measuring tensile, compressive and shear strengths, specific heats and thermal conductivities. The tests were performed on two soils at temperatures from ambient to -195C. Because it is difficult to find data in the literature that pertain to a particular soil, ice was used to evaluate some of the experimental procedures. Some of our ice data are compared to the published values. PHYSICAI, PROPERTIES SOIL SELECTION AND SAMPLE PREPARATIONS The physical and thermal tests were performed on recompacted samples of two typical soils that might be encountered in underground caverns: a gray, fire clay that had been pulverized and mixed with water into a pliable mud; and a brown, sandy silt that was dug from a dry river bank and subsequent1y mixed with tap water. The moisture content of the test specimens was 17 to 22 per cent (based on the wet weight of the soil). This amount of water nearly saturated the silt, but the clay was well below the saturation point. The soils are partially described by the sieve analyses (Fig. 1) which show the particle size distribution of the coarser than 44 micron portion of the soils. The curves also show that approximately 75 per cent of the clay and 20 per cent of the silt are finer than 44 microns. The particle size seems to affect some of the physical properties, and the finer than 44 micron portion is important in the thermal conductivity test. Physical specimens were cut with a bandsaw from frozen blocks of the soil. The specimens were then sanded and kept frozen until after they were tested. They were stored at the approximate test temperature for several hours. Then, to equilibrate the samples to the test temperature, they were stored at the temperature at least an hour before they were tested. TEST EQUIPMENT An Instron, which is a constant speed gear-driven instrument, applied force to the samples and drew stress-strain plots of the test. All of the samples were strained at 0.02 in./min. All of the physical tests were conducted in a temperature cabinet that controlled the temperature to 1C. TENSILE STRENGTH Briquette or "dog-bone" shaped tensile specimens were pulled with suitably shaped jaws. This shape of specimen, which is usually used for tensile tests of concrete, is satisfactory for testing frozen soils except that the samples tend to

Jan 1, 1965

By C. H. Li, R. J. Stokes

This paper compares the fracture behavior of tungsten rods in three conditions: recrystallized. recovered, and wrought. Notched specimens suhjected to a 50 in.-lb impact load showed ductile-brittle transitions at 700, 4.90°, and 440°C, respectinely. The recrystallized material had an equiaxed pain structure and jracbred by simple cleavage from a grain boundary source at all temperatures up to 700°C. The wrought and recovered material had an elongated fibrous structure and at low temperatures fractured by cleavage originating from the notch. As the transition temperature was approached cleavage was preceeded by more and more intergvanular splitting which deflected the crack front into planes parallel to the tensile axis. The enhanced toughness of wrought and recovered tungsten was attributed both to its inability to initiate cleavage because no pain boundaries were suitably oriented perpendicular to the tensile stress and to its inability to maintain cleavage because of intergranular splitting ahead of the crack. It has been appreciated for a long time in a qualitative manner that the room-temperature brittleness of fully recrystallized tungsten may be alleviated by working the material at relatively low temperatures.' More recently this difference in mechanical behavior between wrought and recrystallized tungsten has been examined quantitatively by measurement of the tensile properties as a function of temperature. In these experiments brittleness has been expressed in terms of ductility or reduction in cross-sectional area upon tensile fracture or in terms of the bend radius before fracture under bending.' This work has shown the existence of a fairly sharp transition from brittle to ductile behavior with an increase in temperature. The ductile-brittle transition temperature for recrystallized material is approximately 200°C higher than for wrought material. An increase in strain rate, small additions of impurity,' or an increase in grain size4 shift the respective transition temperatures to higher values, but the difference between them remains approximately the same at 200°C. A number of explanations for this embrittlement by recrystallization have been given. It has been blamed either on the concentration of impurity at the grain boundaries, the increase in grain size, or the change in texture which occurs upon recrystallization. The present paper examines the effect of different heat treatments on the notch-impact behavior of commercial powder-metallurgy tungsten rods. The change in the ductile-brittle transition temperature for this method of loading and the fracture mode has been related to the different mi-crostructures produced by heat treatment. EXPERIMENTAL PROCEDURE Commercial swaged powder-metallurgy tungsten rods 1-3/8 in. in length and 1/8 in. in diameter were machined to introduce a sharp V notch 0.030 in. deep. To change the microstructure from that of the as-received wrought material some of the specimens were subjected to an anneal in nitrogen either at 1300° or 1400°C for 8 hr or at 1600° or 2000°C for 1/2 hr. The notched rods were then placed in a miniature Charpy-type impact machine and struck at their midpoint (opposite the notch) with a hammer designed to deliver 50 in.-lbs of energy. The strain rate at the base of the notch was estimated to be approximately 100 sec-1 at the instant of impact. The specimens were heated in situ to the desired impact temperature. The microstructures produced by the various anneals were studied by both X-ray diffraction and metallographic techniques. Fig. 1 reproduces the microstructures observed metallographically following a 10-sec electroetch in a 10 pct KOH solution. Fig. l(a) shows the elongated fibrous grain structure of the as-received material. Following the anneal at 1300" or 1400°C the grain structure was still elongated as shown in Fig. l(b) but the etch pits delineated dense polygonized dislocation arrays within many of the grains. Occasionally a relatively dislocation-free recrystallized grain was found growing into the matrix. The anneals at 1600° and 2000°C resulted in complete recrystallization and some grain growth. The grains produced at 1600°C were still slightly elongated as shown in Fig. l(c) whereas the anneal at 2000°C produced equiaxed grains. The changes in grain size produced the expected changes in the X-ray back-reflection patterns; there was no indication either in the as-received material or the annealed material of any preferred orientation. RESULTS a) Impact Behavior. Fig. 2 reproduces the ductile-brittle transition curves measured in the manner described in the previous section. It can be seen that under these testing conditions the as-received

Jan 1, 1964

By R. Shuttleworth, R. Smith

A Knudsen effusion tnethod I~as been used lo measure the vapor pressure of pure iron in the temperature range 1000° to 1500°C. Neutron-irradiated , natural iron was used and the Mn'~proclzdced by the (n, p) reaction removed by evaporation at high temperature. The results can be represented by the equation: where pM - 1.088 x 107 atm and T, = 20,890°K. A value of 100.2 kcal per g- atom was obtained for AH;. THE vapor pressure of pure iron in the temperature range 1000" to 1500°C has been measured. Radioactive iron and a Knudsen cell technique were used and the Mn' produced by an (n, p) reaction removed by evaporation at high temperature. From the variation of vapor pressure with temperature values of the enthalpy and entropy of solid iron have been found. Previous workers2 used a Lang-muir method and measurements were made over a smaller temperature range than that in this work. EXPERIMENTAL The apparatus used was similar to that of Pyle and Shuttleworth, and McLellan and Shuttle worth. However, because of the higher temperatures the Knudsen cell was machined from tungsten bar and the flanged furnace tube was beryllia. Heating was by passing a high current (70 amp at 7 v for 1500°K) through a strip of tantalum foil laid across the top of the cell and through a turn of molybdenum wire around the furnace tube. This method of heating ensured that the top of the cell was slightly hotter than the base and prevented condensation and re-evaporation from the orifice. The temperature was measured by means of a pt/Pt 13 pct Rh thermocouple spot-welded to the base of the crucible. To ensure accurate temperature measurement the iron was in the form of a thin disc (0.75 cm diam by 0.075 cm) which lay on the base of the cell. The high-purity iron was irradiated in the Harwell pile for a week at a neutron flux of 1.2 X 10" neutrons per sq cm per sec. The isotopes fe'~ and Fe" are produced by (n! y) reactions but only Fe", half-life 45.1 days, is a emitter; Mn which is also a y emitter, half-life 300 days, is produced simultaneously by an (n,p) reaction.' Immediately after irradiation of natural iron the ratio of ~e" to Mn y activity was 100:l. However, manganese is very much more volatile than iron and almost all the y activity of the condensate is due to Mn'~. Thus it was essential to eliminate all the manganeses before any measurement of the vapor pressure of iron was made and this was done by preliminary heating for 20 hr at 1400°C. For each determination the iron was dissolved from the target with acid and the y activity compared to a known weight of iron. By means of a y-ray spectrometer the y-activity measurements were made at the 1.09-mev peak of the 17e5' spectrum where the background was of the order of 3 cpm. Despite the low specific activity of ~e" a mass of 10- " g of iron could be determined corresponding to a vapor pressure of about l0-'' atm. RESULTS The vapor pressures were calculated from the equation: Where m is the mass of iron effusing in a time t through an orifice of area a2, r is the radius of the target, Z is the distance from the orifice to the

Jan 1, 1965

By D. Harker, E. Epremian

The constitution of the nickel-tungsten system has been studied by a number of investigators, the most recent of which are Ellinger and Sykes.1 On the basis of metallography, electrical resistivity and hardness measurements and some X ray diffraction work, they constructed a consitution diagram (Fig 1). Ellinger and Sykes report a0 for the alpha face-centered cubic phase (nickel saturated with tungsten) as 3.66?.‡ The gamma phase (tungsten saturated with nickel) is given as body-centered cubic, but no value of a. is recorded. At 43 pct tungsten by weight (approximately 20 at. pct) a beta phase is reported, but structure and lattice parameter are not known. Primarily on the basis of metallographic evidence, they conclude that beta is a new phase and rule out the possibility of formation of a superlattice since they- observe a new phase in the microstructure. Grube and Schlecht2 report an ordering reaction in a system similar to the Ni-W (Ni-Mo) and Harker3 has shown that NirMo forms a superlattice upon the pre-existing face-centered cubic lattice of the alpha phase. Elliniger arid Sykes observed a change in the diffraction pattern of a 4.3 pct W alloy upon aging and attributed it to the formation of a new phase. Thus, there appears to be some question as to the character of the beta phase reported by Ellinger and Sykes. The purpose of the present work is to determine precisely the structure and nature of the beta phase in the Ni-w system of X ray diffraction methods. Experimental Procedure One inch diameter ingots of 43.66 pct, 40.15 pct and 34.06 pct .tungsten by weight (19.8, 17.6 and 14.1 at. pct respectively) were melted and cast under vacuum from electrolytic nickel and pure wire filament grade tungsten. The ingots were soaked for 16 hr at 1300°C in a hydrogen atmosphere furnace, then swaged at this temperature and finally drawn to 0.020 in. diam wire. Some of the bar stock was retained in 1/2 in. diam rod for hardness and metallographic studies. Wire samples for diffraction work were sealed in evacuated quartz tubes and subjected to the various solution and aging heat treatments in a hydrogen furnace. X ray photograms were taken in a Debeye-Slierrer camera using copper K radiation filtered by nickel foil. Results X RAY DIFFRACTION The lattice parameters of the alpha and gamma phases at saturation were determined by an X ray photogram of the 19.8 at. pct W alloy after solution heat treatment at a temperature well within the alpha-gamma range above the peritectoid temperature (17 hr at 1150°C—oil quenched). The alpha phase was found to be face-centeted cubic with a. of 3.594 ± 0.001?, while the gamma phase was determined as body-centered cubic with a. of 3.158 ± 0.001?. Exactly the same phases and parameters were ohtained with the 17.6 at. pct W alloy for the same solution heat treatment. Thorough analysis was made of an X ray photogram of a 19.8 at. pct alloy sample in the quenched and aged condition (solution treated 1T hr at

Jan 1, 1950

By F. D. Rosi, C. H. Mathews

THE plastic properties of face-centered cubic metals below room temperature present a field of investigation which has not been extensively ex-plored. The work by Schmid and Boas1 has demonstrated the importance of temperature upon such properties as strain hardening and critical resolved shear stress. The work by Yamaguchi2 upon the shear stress as related to the number of slip bands accentuates the necessity for further experiments of a similar nature. The approach to a mechanical equation of state from the standpoint of thermal fluctuations and activation energies by Becker3 and more recently by Kauzmann4 further emphasizes the need for a quantitative and more comprehensive analysis of the dependence of fundamental plastic properties on temperature. The purpose of the present work was to investigate specifically: (1) The gross shape of the stress-strain curves at several temperatures, (2) the change in the critical shear stress as a function of temperature, and (3) the number and appearance of slip bands as a function of strain and temperature. Preparation of Specimens Single-crystal specimens of 99.996+ pct alumi-num, 1/2 in. in diam and 5 to 6 in. in length, were made by the Bridgman method of gradual solidification from the liquid state. The crystallographic orientation of the single crystals was determined from back-reflection, Laue X-ray photograms ac-cording to the method described by Greninger.6 In most specimens the Laue photograms showed double diffraction spots indicative of the lineage structure type of imperfection, discussed in great detail by Buerger.7 The angular spread of these spots was never observed to exceed 2". Most of the crystals were radiographed to insure against microporosity. In preparing the metal surface for optical microscopy, the following sequence of operations gave good results: The as-cast crystals were turned down in a lathe, 0.001 in. per cut, to obtain a 2.5 in. gauge length. The cold-worked layer resulting from this operation was removed chemically by etching with Tucker's reagent. Then the specimen was polished mechanically through 2/0 metallographic emery paper, after which it was etched again to remove the cold-worked layer resulting from the mechanical treatment. A 48-hr anneal at 580°C ±10°C followed so as to insure an essentially stress-free single crystal. After the annealing treatment, the specimen was electrolytically polished in a 2:l solution of methyl alcohol and concentrated nitric acid. With a current density of 10 amp per sq dm (decimeter) the time required to obtain a satisfactory surface varied from 10 to 12 min. The polish-ing was carried out for short periods of 2 min to avoid rapid deterioration of the solution as well as to enable the rotation of the specimen 180" for uniformity of polish. It was necessary to place the solution in a bath of dry ice in view of its explosive nature at room temperature. Etching of the electrolytically polished surface was accomplished by using the fuming etch-pit method recommended by Lacombe and Beaujard8 for high-purity aluminum. Method for Tensile Testing A modification of the loading equipment devised by Miller9 was used. In this apparatus, the specimen was suspended from a chain and gimbal arrangement (for axial loading) in a heavy steel framework connected at the bottom to a balanced 6:1 lever and bucket system. Loading of the specimen was accomplished by allowing sand to flow from a reservoir into the bucket suspended from the longer end of the lever-arm at a rate of approximately 3 lb per min. Strain measurements were made using the Baldwin SR-4, bonded, resistance-wire, strain gauge and an SR-4 portable strain indicator (type K), which permits a reading accuracy of 2 microinches per inch. For low-temperature study, the gauge was calibrated by measuring the elastic modulus of an annealed stainless steel rod, which is known to be independent of temperature."

Jan 1, 1951

1. Healthy and active Local Section organizations are vital factors in promoting the vigor and growth of the Institute. 2. Activity on the part of Local Sections should be recognized and stimulated by appropriation of funds from the Institute's treasury; and these appropriations should be as large as is consistent with the relative needs for other activities. 3. As between different Sections, the amount of such appropriations should be based primarily on the extent of activities as reflected in the number and character of meetings held and " the attendance of the members at such meetings. 4. In making a request for funds for any year, the officers of a Local Section should submit a report on the printed form approved by the Directors at their meeting on November 19, 1937. 5. A standing Committee on Local Section Appropriations, consisting of one past chairman of a Local Section, one member of the Institute's Executive Committee, and one member of the Finance Committee, shall be appointed by the President and shall pass upon requests for appropriations and authorize payments within bounds of the budget. The committee will be guided by the principles herein outlined, always having in mind the vital importance of healthy, active Sections to the welfare of the Institute as a whole. 6. According to Article XI, Section 2 of the Bylaws, requests for appropriations shall be signed by the Chairman, Secretary and Treasurer of the Section. 7. Requests for appropriations must be in the hands of the Secretary of the Institute by February 15 of the year for which they are desired.

Jan 1, 1940

1. Healthy and active Local Section organizations are vital factors in promoting the vigor and growth of the Institute. 2. Activity on the part of Local Sections should be recognized and stimulated by appropriation of funds from the Institute's treasury; and these appropriations should be as. large as is consistent with the relative needs for other activities. 3. As between different Sections, the amount of such appropriations should be based primarily on the extent of activities as reflected in the number and character of meetings held and the attendance of the members at such meetings. 4. In making a request for funds for any year, the officers of a Local Section should submit a report on the printed form approved by the Directors at their meeting on November 19, 1937. 5. A standing Committee on Local Section Appropriations, consisting of one past Chairman of a Local Section, one member of the Institute's Executive Committee, and one member of the Finance Committee, shall be appointed by the President and shall pass upon requests for appropriations and authorize payments within bounds of the budget. The committee will be guided by the principles herein outlined, always having in mind the vital importance of healthy, active Sections to the, welfare of the Institute as a whole. 6. According to Article XI, Section 2 of the Bylaws, requests for appropriations shall be signed by the Chairman, Secretary and Treasurer of the Section. 7. Requests for appropriations must be in the hands of the Secretary of the Institute by February 15 of the year for which they are desired.

Jan 1, 1946

1. Healthy and active Local Section organizations are vital factors in promoting the vigor and growth of the Institute. 2. Activity on the part of Local Sections should be recognized and stimulated by appropriation of funds from the Institute's treasury; and these appropriations should be as large as is consistent with the relative needs for other activities. 3. As between different Sections, the amount of such appropriations should be based primarily on the extent of activities as reflected in the number and character of meetings held and the attendance of the members at such meetings. 4. In making a request for funds for any year, the officers of a Local Section should submit a report on the printed form approved by the Directors at their meeting on November 19, 1937. 5. A standing Committee on Local Section Appropriations, consisting of one past Chairman of a Local Section, one member of the Institute's Executive Committee, and one member of the Finance Committee, shall be appointed by the President and shall pass upon requests for appropriations and authorize payments within bounds of the budget. The committee will be guided by the principles herein outlined, always having in mind the vital importance of healthy, active Sections to the welfare of the Institute as a whole. 6: According to Article XI, Section 2 of the Bylaws, requests for appropriations shall be signed by the Chairman, Secretary and Treasurer of the Section. 7. Requests for appropriations must be in the hands of the Secretary of the Institute by February 15 of the year for which they are desired.

Jan 1, 1946

By A. H. Daane, B. J. Beaudry

The Sc-Y and Sc-Zr systems were studied by thermal and X-ray methods. Both systems are characterized by complete solid solubility in the low temperature hexagonal form and in the high temperature bcc form. In the Sc-Y system, there is a minimum in the solidus at 50 at. pct and 1365°C, while the solidus in the Sc-Zr system follows a nearly straight line relationship between the melting point of scandium and zirconium. There is a minimum in the temperature of transition from hexagonal to bcc in the Sc-Y system at 43 at. pct Y and 1175°C; while the temperature of transition is raised in the Sc-Zr system to a maximum of 1415 °C at 30 at. pct Zr. INTEREST in the metals of the first transition series has usually stemmed from their useful properties; however, there is now a great deal of interest in determining the fundamental nature of these metals. Since scandium is the first of these transition metals, a study of the preparation and Properties1 and the alloying behavior of scandium2 was initiated. In a continuing study of the alloying behavior of scandium, the systems of scandium with zirconium and yttrium have been established. Extensive solid solubility in both the Sc-Zr and Sc-Y systems was expected from application of the classical rules of Hume-Rothery. Also, the modified Darken and Gurry plot as suggested by Gschneid-ner3 showed ideal conditions for solubility in the Sc-Zr system with less favorable conditions in the Sc-Y system. The effect of scandium on the transformation temperature of zirconium and yttrium was of interest, since a recent empirical observation by Uly and Burr4 predicted that the solute scandium would raise the transformation temperature of zirconium and lower the yttrium transformation. In addition to noting the validity of the above predictions, the SC-Y and Sc-Zr systems were established. EXPERIMENTAL METHODS Materials. The metals employed in this investigation were crystal bar zirconium, distilled scandium prepared by the method described by Spedding, et al.1 and yttrium prepared by the method described by Carlson, et a1.5 The major impurities present in these metals are listed in Table I in ppm. Alloy Preparation. All the alloys examined were initially formed by comelting the two metals in a nonconsumable electrode arc-melting furnace under an atmosphere of purified helium or argon. The buttons were inverted at least five times and re-melted each time to ensure homogeneity. During preparation of Sc-Zr alloys, approximately 1 wt pct was lost which was attributed entirely to the loss of scandium by distillation. When preparing Sc-Y alloys, approximately 1.5 wt pct was lost, but it was assumed that the intended composition was maintained, since the relative weight lost when arc melting the component metals was nearly the same. Samples weighing 15 to 20 g were prepared for time-temperature thermal analysis, while only 1- to 2-g samples were prepared for the optical pyrometer and X-ray diffraction studies. Thermal Methods. The solidus and the melting points of the metals were determined by an optical pyrometer method described previously.2 The temperatures at which the transformation from hexagonal to bcc occurs were determined by differential thermal analysis. Several points on the solidus and liquidus in the Sc-Y system were also determined by this method and are in good agreement with those obtained by the optical pyrometer method. The procedure followed in the preparation of samples for thermal analysis and the furnace used have been described elsewhere.2'6 Since a limited quantity of scandium was available, most of the alloys were not melted during thermal analysis, thus avoiding contamination by the crucible. The alloy could then be reused and the composition changed by adding the desired quantity of solute to obtain the next alloy. Heat Treatment and X-Ray Methods. In order to ensure homogeneity, the "as arc-melted" alloys Were wrapped in tantalum foil, sealed in quartz capsules and heated at 1100°C for 15 hr and then cooled at a rate of 8 deg per min. Samples for X-ray diffraction were filed from these heat-treated alloys, sealed in 1/8 in. by 1/2 in. tantalum capsules under

Jan 1, 1963

By R. P. Aikman, F. G. Miller, J. M. Podgursky

In response to the growing demand for low-sulfur coking coal for iron-making, the coal industry is continually striving to perfect methods for cleaning coal to acceptable ash and sulfur levels while maintaining maximum product yield. By present standards the industry has adequate processes for cleaning coarse coal, (i.e., +28 mesh) at almost any desired specific gravity. However, in the case of fine coal (i.e., -28 mesh) neither of the two existing processes-froth flotation and hydrocycloning-in its present state of development yields products that are comparable in ash and/or sulfur content to products normally obtained from coarse coal processes. The work outlined in this article is part of a larger study directed toward maximum exploitation of froth flotation for fine coal processing. The concepts and data presented are now serving as a basis for designing fine-coal circuits in which improved efficiency is obtained by optimum use of froth flotation with other fine-coal processing methods.

Jan 7, 1967

T. L. Joseph (University of Minnesota, Minneapolis, Minn.)—Mr. Killian is to be commended for his inquiry as to why a decrease of 15.3 pct in coke consumption was accompanied by a decrease of only 1.9 pct in the CO/CO, ratio of the top gas. Although I encouraged him in his efforts to find a more significant and meaningful carbon-gas ratio, the method, calculations, and conclusions originated entirely with the author. Whether we agree entirely with the assumptions underlying his corrected ratio, I think we can all agree that a better ratio is needed, and that he deserves credit for recognizing the need and for doing something about it. To be most useful, the CO/CO, ratio for the top gas should reflect the way in which the carbon is gasified in the furnace, particularly the degree of oxidation and the extent of heat release. The effect of CO, from the decomposition of the limestone and the effect of the reaction of CO and water vapor in the upper part of the furnace on the quality of top gas should be isolated from the effect of more basic reactions such as ore reduction and solution loss. The reduction of sufficient iron oxide to produce a ton of pig iron and the accompanying changes in the proportions of the carbon gases can be expressed on a mol basis as follows: 16.5FeA + 16.5CO - 33FeO + 16.5CO, [1] 33FeO + 33.0CO = 33Fe + 33CO. [2] The CO, from eq 1 normally escapes from the furnace because it does not react with coke at the temperature of its release. However, as much as 50 pct of the CO, from eq 2 may react with coke because it is released at temperatures above 1000°C: 16.5CO. + 16.5CO2 = 33CO [3] Thus we see that the gasification of 16.5 mols or about 200 lb of C in solution loss will regenerate as much CO as is required for the last stage of reduction. The pronounced effect of reaction 3 on the final proportions of CO and CO, in the gas stream is obvious. It also follows that reaction 3 materially alters the heat release but it cannot be entirely eliminated in Lake ore practice. A previous study indicates that 100 lb of solution loss may be necessary to maintain the reducing power of the gas. A reduction of 100 lb from the normal level of 200 lb would mean that over 1,-000,000 additional Btu are released in the process. The 100 lb of additional carbon which will be burned at the tuyeres will release 437,000 Btu and the absorption of 583,000 Btu by eq 3 would be prevented. One of the chief objectives of sized ore burdens and more uniform distribution of the gas stream is to minimize solution loss by completing reduction higher in the furnace and in turn to release the maximum amount of heat from the carbon charged. It was odd, indeed, to find that the use of sized ore and sinter in the careful tests reported by Dobscha had changed the CO/CO2 ratio very little. The author has stressed the close correlation between his corrected CO/CO, ratio and production. A correlation of fuel consumption and the CO/CO, might be more logical. Fuel consumption on the prepared ore burden decreased 15.3 pct whereas the corrected CO/CO2 ratio decreased 19.0 pct. Although this agreement between the reduction in fuel and the reduction in corrected CO/CO2 ratio is not as close as the correlation with tonnage, it indicates the corrected ratio is superior to the normal ratio which decreased less than 4 pct. Some adjustment should be made for the reaction: CO + H2O = CO2 + H2 —700Btu [41 because there is evidence to indicate that about one half of the hydrogen is formed in the upper 21 ft of

Jan 1, 1953

By J. S. Marsh, T. B. Winkler

THE past year, the first full one of peacetime production, proved that the process of beating swords into plowshares has increased in complexity in step with civilization. Further, judging by various remarks of our distaff departments, the crystal balls of certain radio and magazine oracles must have been cloudy, because we have been in formed from time to time that coveted items such as automobiles and refrigerators did not appear in great abundance. This seemingly extraneous matter is really not out of place here, however; the steel producer and the fabricator exist in a sort of symbiosis: the making of consumer goods produces scrap which is returned to the steelmaker who makes more steel, and so on and so forth. Thus, no abundance of automobiles, no abundance of scrap from this normal source; and other sources had been picked pretty clean during the war. To be short, so was scrap. Since the economy of the steel industry lean; as heavily upon iron from scrap as upon iron from ore, the statement on transformation of swords to plowshares follows. But this is not the whole story: after all, ingot production was a record for a peace year!

Jan 1, 1947

By Earl S. Greiner, Eric R. Jette

ALTHOUGH the mechanical and chemical characteristics of certain iron-nickel-silicon alloys have been investigated,1 the available literature shows no results of a systematic investigation of the constitution of this system. This paper describes the results of an X-ray investigation of the constitution of the iron-rich iron-nickel-silicon alloys at 600°C. Data on the constitution of the included binary systems obtained in other investigations have been correlated with the structure of the ternary alloys. Jette and Foote2 have presented a tentative constitutional diagram of the iron-nickel system following X-ray studies on quenched specimens. This diagram shows that the alloys at 600°C. containing from zero to approximately 4 atomic per cent nickel consist of a body-centered cubic (alpha) phase, the alloys containing 4 to 24 atomic per cent nickel consist of body-centered cubic (alpha) and face- centered cubic (gamma) phases, and the alloys containing from 24 to 100 atomic per cent nickel consist of a face-centered cubic (gamma) phase. These investigators recognized that it was not possible to retain the gamma phase in equilibrium by quenching alloys containing less than approximately 25 atomic per cent nickel and that high-temperature X-ray methods were desirable to determine the gamma-phase solubility limit. In a later investigation of the iron-nickel alloys, Owen and Sulley3 determined the alpha-phase solid solubility limit to be 3.5 atomic per cent nickel at 600°C. High-temperature X-ray methods showed the solid solubility limit of the gamma phase to be 14 atomic per cent nickel at 600°C. Since the high-temperature X-ray method should reveal equilibrium conditions in these alloys better than the quench method of other investigators, the results of Owen and Sulley pertaining to the gamma-phase boundary are to be preferred. As the result of an X-ray investigation of quenched iron-silicon alloys, Greiner and Jette4 have shown these materials to consist of a body-centered cubic (alpha) phase containing from o to 26.4 atomic per cent silicon at 600°C. The alloys containing from 26.4 to approximately 50 atomic per cent silicon consist of two phases at 600°C.; namely, alpha and eta. The eta phase corresponds to the stoichiometrical formula FeSi (33.4 wt. per cent Si).* The literature pertaining to the constitution of the nickel-silicon alloys has been reviewed by Ackerman,5 who found disagreements in the results of various investigators on several parts of the system. Subsequent data on the constitution of the nickel-silicon alloys were reported by Osawa and Okamoto.6

Jan 1, 1943

By AIME AIME

THE technical material in hand and the plans under way for the 141st meeting of the Institute clearly indicate a well-rounded program of unusual excellence. The meeting will be held in the Engineering Societies Building, Feb. 15 to 18, and while it is too early to announce definitely the time of the various sessions much of the detail has been organized up to that point. Every group in the Institute membership will find much of special interest, and several features should prove generally attractive. The various committees in charge of the lighter side of the meeting are hard at work to emulate the standard established last February In this connection and in this paragraph it will suffice to say-there will be a Smoker-dinner! The Committee on Mining Methods plans two sessions for which these papers are in prospect:

Jan 1, 1932