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By A. Steiner, K. L. Komarek

Activities of aluminum in solid Ni-A1 alloys have been determined between 20 and 60 at. pet Al and 1200" and 1400°K by an isopiestic method in which nickel specimens, heated in a temperature gradient, are equilibrated with aluminum vabor in a closed all-alumina system. The activity of aluminum shows a strong negative deviation from Raoult's law at low concentrations but increases by three orders of magnitude within the ß(NiAl) phase. The partial molar enthalpy and entropy of mixing are negative. Using Wagner and Schottky's theory of ordered compounds, a degree of disorder of 4 x 10 -4 for NiAl and 1.25 X 10-2 for FeAl has been calculated THE Ni-A1 system has been studied by a great number of investigators, and the results, as far as the phase diagram is concerned, have been compiled by Hansen.1 The phase boundaries from 0 to 50 at. pet Ni are well-established. At higher nickel contents the boundaries are still in dispute and an additional phase, A12Ni3, has been reported.' The phase diagram is dominated by a very stable high-melting compound, NiA1, with a relatively wide range of homogeneity. Heats of formation of solid alloys have been determined calorimetrically by Oelsen and Middel3 from 20 to 95 at. pet Ni and by Kubaschewski4 from 25 to 80 at. pet Ni. According to the most recent compilation5 no other thermodynamic investigations have been reported for the Ni-A1 system. Due to the corrosive nature and the low vapor pressure of aluminum, a method has been employed for determining activities of aluminum which was previously developed for the Fe-A1 system.= Nickel specimens, heated in a closed evacuated alumina system in a temperature gradient, were equilibrated with aluminum vapor from a source within the system kept at constant temperature. After complete equilibration the specimens were analyzed and activities calculated from the known vapor pressure of aluminum. APPARATUS AND EXPERIMENTAL PROCEDURE Materials. The nickel specimens were made from wafers of electrolytic nickel (International Nickel Corp.) of 99.99 pet purity which were rolled to a 0.001-in.-thick foil by Driver-Harris Co. and to a 0.005-in.-thick sheet in our laboratory. The aluminum (Aluminum Corp. of America) had a purity of 99.99+ pct. The alumina tubes and crucibles were made of impervious recrystallized alumina with an alumina content of 99.7 pet (Triangle RR, Mor-ganite Inc.). Experimental Procedure. Annular specimens were punched from the sheet, the punching burrs removed, and the specimens degreased in carbon tetrachloride and acetone and weighed on a micro-balance to within an accuracy of ±0.01 mg. The specimens were positioned with alumina spacers along an alumina tube, and the positions measured. Aluminum metal was machined into cylindrical shape, and placed into an alumina crucible. The tube with the specimens was then inserted into a hole drilled into the aluminum metal. An alumina tube with its closed end at the top was slipped over the specimens so that its lower end fitted snugly into the alumina crucible. The assembled reaction tube was inserted into a mullite tube with a water-cooled brass head which had an opening for a quartz thermocouple protection tube and a metal-to-glass connection to a conventional vacuum system. A Pt-Pt 10 pet Rh thermocouple could be raised and lowered in the quartz tube which was placed along the outside of the alumina reaction tube. The mullite tube was heated by two separately controlled resistance-tube furnaces so that in the experimental temperature range an over-all temperature gradient of approximately 150o to 250°C could be imposed on the reaction tube. The position of the mullite tube was adjusted so that the surface of the aluminum metal was always at the temperature minimum. The reaction tube was thoroughly evacuated before and during slowly heating the assembly up to the melting point of aluminum. A pressure of less than 2 µ (Hg) was maintained during an experiment. Once the aluminum had melted, it isolated the contents of the alumina tube from the surroundings. Several times during an experiment the temperature gradient was carefully measured. An experiment lasted from 3 to 6 weeks and it was terminated by air cooling the evacuated mullite tube. For further details of the experimental procedure the paper on the Fe-A1 system6 should be consulted.

Jan 1, 1964

By H. C. Gatos, J. T. A. Pollock

It is well known that the superconducting critical current densities of many alloy superconductors may be increased by cold working and in some cases further enhanced by a short heat treatment. This latter enhancement has been attributed to the redistribution of dislocations into cell-like networks' and to the precipitation of second phase particles,2'3 which act as flux pinning centers. In a manner analogous to dislocation pinning in precipitation hardening alloys,4 it is expected that here also a critical distribution of the pinning centers should result in maximum pinning effect. Concentration inhomogeneities exist in most or all commercial alloys yet there have been only a few attempts made to determine their effect on critical current capacity in the absence of cold working. Sutton and Baker,5 and Kramer and Rhodes6 have found that the complex precipitation processes occurring during the aging of Ti-Nb alloys can result in critical current density enhancement. Livingston7-10 has clearly shown, for lead and indium based alloys, that the distribution of precipitated second phase particles is of critical importance in determining magnetization characteristics. However, these '(soft" alloys age at room temperature and the time involved in specimen preparation prevents metallographic examination in the state in which the superconducting measurements are made. Thus results with such alloys are expected to be biased towards larger precipitates and interpar-ticle spacing. The present study of Ta-Zr alloys was undertaken to examine the influence of second phase precipitation, as controlled by heat treatment, on the critical current capacity of well annealed polycrystalline material. A study of the published phase diagram11 indicated that annealing supersaturated samples containing up to 9 at. pct Zr at suitable temperatures would result in the precipitation of a zirconium-rich second phase. It was MATERIALS AND PROCEDURE The alloys were prepared from spectrochemically pure tantalum and zirconium. Analysis was carried out by the supplier. Major impurities in the tantalum were: 12 pprn of 02, 17 pprn of N2, 19 pprn of C, and less than 10 ppm each of Mo, Nb, Al, Cr, Ni, Si, Ti. The crystal bar zirconium was pure except for the following concentrations: 15 pprn of 02, 17 ppm of C, 23 ppm of Fe, 11 ppm of Cu, and less than 10 pprn each of Al, Ca, N2, Ti, and Sn. Samples were prepared in the form of 8 to 10 g but-tons by arc melting using a nonconsumable electrode on a water-cooled copper hearth in a high purity ar-gon atmosphere. Each button was inverted and re-melted three times to ensure an even distribution of the component elements. The samples were then homogenized at temperatures close to their melting points for 3 days in a vacuum furnace maintained at 5 x 10-7 mm Hg. After this treatment the buttons were cold rolled to sheets approximately 0.020 in. thick from which specimens were cut, 0.040 in, wide and 1 in. long suitable for critical current density (J,) and critical temperature (T,) measurements. These strips were then recrystallized and further grain growth was allowed by an additional vacuum heat treatment at 1800°C for 60 hr. Some second phase precipitation occurred during cooling of the furnace and a solution treatment was necessary to produce single phase supersaturated samples. This treatment was successfully carried out by sealing the samples together with some zirconium chips in quartz tubes under a vacuum of 5 x 10-7 mm Hg, heating at 1000°C for 5 hr and then quenching into water or liquid nitrogen. The samples were then heat treated at either 350" or 550°C and quenched into water or liquid nitrogen. All samples which were heat treated at 350°C were quenched in both cases by cracking the capsules in liquid nitrogen. The samples treated at 550°C were quenched by dropping the capsules into water. Analysis for oxygen in randomly selected samples indicated that the oxygen content was in the range of 175 to 225 ppm. Values of Tc were determined by employing a self-inductance technique. Jc measurements were made at 4.2oK by increasing the direct current through the wire in a perpendicularly applied field until a voltage of 1 pv was detected with a null meter. The risk of resistive heating at the soldered joints during these latter measurements was reduced by first plating the ends of the wires with indium and then soldering to the copper current leads using tin. Metallographic examinations were performed after mechanical polishing of the same samples and etching in a 4H20:3HN03 (conc):lHF(conc) solution.

Jan 1, 1970

By H. R. Green, D. M. Lamb, A. D. Taylor

The design of slurry launders has usually been based on strictly empirical concepts. An examination of the most common procedures reveals that they do not account for many of the variables that are recognized as significant for slurry transport. These may include flow rate, volume concentration of solids, solids specific gravity, solids size distribution, particle shape, launder geometry, and roughness of the wetted surface. It was decided to develop a design procedure, which would accomplish two things:

Jan 8, 1978

By E. M. Wise

THE practice of adding moderate quantities of nickel to a variety of bronzes has been employed by foundrymen for many years with several objects in view. In some instances it was desired- to harden the alloy; in others it was to increase the fluidity or to improve the solidity of the castings, or to refine their grain. These important matters have been considered in detail by Pilling and Kihlgren1 and by numerous other workers cited by them, and with the exception of the first will not be considered in the present communication. The possibility of reducing the cost of bronze by replacing a portion of the tin with nickel received attention some years ago by Burgess and Woodward,2 and, as will be shown later, offers attractive savings in cost under present conditions. The age-hardening characteristics of the nickel bronzes of appropriate compositions have been known for some time and were mentioned by Price, Grant and Phillips3 and discussed by Wise4 in connection with their paper. These matters are further considered in recent patents,5 and are becoming of commercial importance in the production of high-strength castings.

Jan 1, 1934

By Irving Cadoff, Kurt Komarek, Edward Miller

Barium can be purified by equilibration with titanium. The melting point of barium was found to be 726.2° i 0.5 °C. The room-temperature lattice parameters of BaTe and Bask are 7.004 * 0.002A and 6.600 * 0.002A. Melting points for BaTe and Base were found to be 1510° * 30°C and 1830° ± 50°C, respectively. HIGH-purity barium and its compounds are difficult to prepare because of the reactivity of barium with the atmosphere and the large heats of formation of the compounds. Purification of barium by vacuum distillation,' and the preparation and properties of barium oxide2 and barium sulfide3 have been reported. However, little has been done on the homologous compounds barium selenide and telluride. PURIFICATION OF BARIUM Distilled barium obtained from King Laboratories was used as the starting material. The analysis supplied with the metal showed the presence of: 0.4 wt pct Sr, 0.001 pct Mg, 0.02 pct F, 0.003 pct Cu, 0.005 pct Na and less than 5 x 10-3 wt pct of any other metallic impurity. Analyses for oxygen and nitrogen were not available. Since there is evidence4 that any barium nitride present in the starting material may decompose on distillation producing nitrogen which can contaminate the distillate, further purification was performed. At elevated temperatures, any nitrogen and oxygen present in barium should be removed by reaction with titanium. Assuming that the solubility of oxygen in liquid barium is negligible near the melting point of barium, any oxygen present will be in the form of BaO. Removal of oxygen from molten barium is expressed by the equation: BaO(S)+ TixOy(S) = Ba(l)+ TixO(y+1)(s) where Ti,Oy and TixO(y+1) are solid solutions of oxygen in titanium. At 1000°C, the change in free energy for this reaction is negative for (y+1)/x +y+1) x (100) 17.5 at. pct O.5 Since reaction with commercially pure titanium (containing 0.07 wt pct oxygen) results in a free energy change for the reaction of -19 kcal per g-atom, slight solubility of oxygen in barium would not hinder the oxygen removal. Since comparable thermodynamic data are not available to permit calculation of the partition of nitrogen between liquid barium and titanium, a similar quantitative relationship cannot be obtained. However, on the basis of work by Kubaschewski and Dench,5 complete removal of nitrogen from liquid barium can be expected. Since the melting point of barium is depressed markedly by small additions of nitrogen,' the change in melting point during reaction of barium with titanium was used to follow the purification reaction. MELTING POINT OF BARIUM A 50-g sample of barium was sealed by arc welding under argon into an all titanium crucible provided with a thermocouple well. The melting point of the sample was determined by thermal analysis, using a Pt/Pt-10 pct Rh thermocouple which was calibrated according to National Bureau of Standards specification6. The crucible was then heated for 48 hr at 950°C in vacuum and the melting point redetermined. This procedure was repeated until three successive thermal analyses agreed within ±0.5oC, the limits of error of the analysis. The melting point increased from an initial value of 720.0°C to a final value of 726.2°C. Analysis on samples quenched from 950°C gave a solubility value of 0.004 wt. pct Ti. Assuming that the titanium-barium phase diagram is similar to those of titanium-magnesium7 and titanium-calcium,8 the solubility of titanium in liquid barium decreases with decreasing temperature. Therefore, the solubility of titanium in liquid barium should be less than 0.004 wt. pctat the melting point (726oC), and the effect of dissolved titanium on the melting point would be negligible. Addition of up to 3 wt pct Sr does not significantly change the melting point of barium,7 so that the effect of the 0.4 wt pct Sr in the starting material will also be negligible. The value of 726.2" ± 0.5C obtained for the melting point of barium can be compared .with a determination carried out by Keller and coworkers in low-carbon steel crucibles,' who obtained a value of 725± 1C, using barium purified by fractional distillation. The higher value obtained in the present investigation is indicative of the effectiveness of titanium in removing traces of nitrogen. PREPARATION OF BaTe AND Base The compounds were prepared by direct reaction

Jan 1, 1961

By W. E. Quist, R. Taggart, D. H. Polonis, C. J. van der Wekken

An intermediate compound that has been identified as Niab is observed to form as a decomposition product from supersaturaled Ni-Nb solid solutions during aging at temperatures between approximately 300" and 500°C. On the basis of data from electron microscopy and selected-area diffraction, the structure of this compound has been determined as fct with a = b - 3a0 and c = a, wlzere a,, is the lattice parameter of the parent solid solution. The compound consists of close-packed layers with triangular ordering, where the niobiutrl atoms are separated by two nickel atoms ([long- close?-packed directions. A nine layer stacking sequence is required to describe the proposed structure. STUDIES of the Ni-Nb binary system have been limited primarily to phase diagram determinations,'-4 investigations of high-temperature equilibrium phases,5"1 and the determination of the influence of deformation on the structure of the equilibrium compound.8 The nickel-rich portion of the binary system is reported to be of the simple eutectic type in which the maximum solubility of 12.7 at. pct Nb occurs at 1282"c.' The two-phase field below the eutectic temperature is bounded by the a fcc solid solution and an orthorhombic Ni3Nb compound. No metastable phases have been reported in previous investigations. In transformation studies of certain nickel-base commercial alloys that contain niobium, two ordered metastable compounds containing niobium have been shown to precipitate from the solid solution, both of which have been identified as y' and have the composition NisNb or Ni,Nb. One compound has been reported to have the bct DOz2 type Al3Ti structure" and the other the cubic LI2 type Cu3Au structure.9,11 In the present work on Ni-Nb binary alloys a metastable y' compound has not been detected after conventional quenching and aging treatments. An anomalous behavior was noted in electrical resistivity measurements. in alloys containing between 7 to 12 at. pct Nb when aging treatments were performed below 500°C after fast quenching from 1250°C. Transmission electron microscopy has shown that this behavior is caused by the formation of a low-temperature precipitate of unreported structure type and composition. EXPERIMENTAL METHODS Several Ni-Nb alloys, containing up to 11.5 at. pct Nb. were prepared by either levitation melting and casting in copper molds or by induction melting in alumina crucibles; both techniques employed purified helium gas as a protective atmosphere. The purity of the nickel and niobium used to make the alloys was 99.98 wt pct Ni and 99.9 wt pct Nb. The composition and homogeneity of the alloys were checked by weight measurements and by electron microprobe analysis. The induction-melted alloys were homogenized for 100 hr at 1100°C. The resistivity specimens were prepared from rods swaged to 2.5 mm and the electron microscopy specimens were cut from sheet that was rolled to 0.4 mm and thinned using a modified Bollmann technique." The elevated-temperature solution treatments were carried out in a purified helium atmosphere followed by direct quenching into a 10 pct NaCl solution at 23°C. Additional protection against oxidation of the samples during solution treatment was accomplished by using tantalum foil as a "getter" in the furnace. The specimens were aged at various temperatures in salt baths controlled to +2oC. A Leeds and Northrup K5 potentiometer was used to make electrical resistivity measurements on specimens immersed in liquid nitrogen. Electron microscopy and diffraction studies were carried out with JEM-7 and Philips EM-200 microscopes operating at 100 kv. RESULTS AND DISCUSSION Ni-Nb alloys containing between 7 and 11.5 at. pct Nb that have been solution-treated in the range 1220" to 1280°C and quenched to 23°C undergo a precipitation reaction when aged in the temperature range 300" to 500°C. Precipitation was detected by selected-area electron diffraction after aging a specimen for as little as 30 sec at 350°C) whereas the reaction was well-advanced after aging for 150 hr at 475°C. Electrical resistivity measurements were used to monitor the progress of the precipitation reaction. In the present experiments the nucleation process for precipitation required a high solution temperature and a rapid quench into brine. The presence of aluminum, iron? and carbon in amounts totaling less than 1 wt pct was found by electron diffraction to completely suppress the formation of the low-temperature precipitate that has been detected in the binary alloy. Electron diffraction techniques were used to determine the structure of the precipitates that formed during the decomposition of the Ni-Nb supersaturated solid solutions. Figs. l(a) through l(d) show electron diffraction patterns oriented to the [loo], [110], [lll], and [I031 zone axes of the matrix. Areas of reciprocal space between these sections were investigated by slowly varying the orientations of the crystal under study; this procedure revealed no reflections other than those depicted in Fig. 1. The presence of super-lattice reflections at points coincident with the matrix reflections was confirmed by the examination of an almost completely transformed structure. On the basis of the accumulated diffraction data, the reciprocal lat-

Jan 1, 1970

By J. Norman Bulkley

As electrical power is used to a greater extent on the Rand than in any other mining center, it is thought that a short description of the methods used and results obtained may be of interest. In comparing Rand practice with that on other fields, several general factors should be borne in mind: First, the mines are all working on large tonnages of low-grade ore (average. $6.50). The annual crushing rate is about 27,000,000 tons. Second, the mines are all grouped udder the financial and engineering control of mining houses, so that the results of a group, rather than an individual mine, are open for study, and practice follows more uniform lines. Third, coal of fair quality (about 12,000 B.t.u.) can be obtained for $2 to $3 per ton., Good supplies of condensing water are, however, scarce, and have to be carefully stored. Power Supply Power is supplied by the Victoria Falls & Transvaal Power Co., Ltd., and its subsidiary, the Rand Mines Power Supply Co. Both companies, which are practically one from an engineering point of view, operate the following stations, all feeding into the same system.

Jan 2, 1916

By Robert B. McCormick

WORLD WAR II has developed a use for the nonmetal mineral quartz crystal that was unknown in World War I. During the interim period of peace, experimental work in the radio field with the piezoelectric properties of quartz crystal resulted in the almost universal adoption of quartz-crystal radio oscillator plates to control frequency in radio broadcasting, police, commercial and amateur communications equipment. Telephone resonators and filters made from quartz crystal also were developed, which vastly improved the frequency control of long distance telephone circuits. EXPANSION OF THE INDUSTRY The sudden war demands of the armed services for radio equipment using quartz crystal for frequency control led to an unprecedented expansion of the manufacturing industry. It is estimated that the 1940 peacetime volume amounted to approximately $1,500,000, while today a vast new quartz-crystal industry supplies more than $150,000,000 worth of quartz oscillator plates to the Army and Navy each year. This demand has caused an enormous expansion not only of American manufacturing facilities but also of Brazilian mining output, virtually our only source of raw quartz crystal. Actual figures of imports and consumption cannot be cited, for security reasons, but certain comparisons have been made, which indicate the transformation of quartz crystal from a minor to a major nonmetal. Lends has shown that the value of quartz-crystal exports from Brazil is now about equal to that of phosphate rock produced domestically in 1941 and actually exceeds the combined value of crude feldspar, gypsum and fluorspar production in the United States in the same year. This great expansion under wartime pressure was not accomplished without some anxious moments, but all the demands of industry have been met and the Government has been able also to accumulate a substantial stock pile of material against future contingencies. INSPECTION AND GRADING OF QUARTZ CRYSTAL The swift growth of the quartz-oscillator industry necessitated the simultaneous evolution of methods and criteria for inspecting and grading quartz crystal. It has been found that, generally speaking, it is economically feasible to cut only crystals that are at least 30 per cent by volume free from major defects such as optical and electrical twinning, cracks and fractures. Blue needles, bubbles, "chuva" and other minor imperfections can be tolerated in the usable portion unless present in great excess. The present marketing system in use in both Brazil and the United States, as far as quality is concerned, depends solely on the "usability" of a crystal, which is defined in the Brazilian-American agreement2

Jan 1, 1945

By K. Winterton

The effect of a near-saturation unidirectional magnetic field was to decrease slightly the endurance life in Armco iron in the annealed condition. This is expected since the energy-absorbing mechanism associated with domain wall movemenfs is inhibited bv the strong field. THE factors determining failure under dynamic loading are not yet clearly recognized. One of the properties of a metal which might be thought to influence fatigue life is its damping capacity. Foppl1 conducted an alternating torsion test at a frequency of 700 cpm continuously for a period of 3 years, without the test piece breaking or showing any sign of deterioration after 1100 Million cycles of stress; the rate of dissipation of energy was sufficient to maintain the test piece at about 100°C above the ambient temperature. cazaud2 concludes from this, and others follow him, that ('the capacity for dissipation in the form of heat by internal damping is unlimited" and that therefore "damping is not directly related with fracture by fatigue." Future work may necessitate qualification of this rather uncompromising view. It is shown later that in all

Jan 1, 1960

By J. J. Gilman

IT is well established that dislocations exist in crystals and account for crystal plasticity.' However, the origins of the dislocations are not clear. Among the means by which dislocations might originate are: a) through crystal growth accidents, b) by the collapse of condensed sheets of vacancies, or c) by stress-induced nucleation. Theoretical calculations' have indicated that the last means should require very high stresses in order to operate. The purpose of this paper is to show that the stresses around the tips of cracks are large enough to nucleate large numbers of dislocation loops. Specifically, it will be shown that (100) cleavage cracks in LiF crystals nucleate dislocations in regions of the crystals where dislocations did not exist previously. It is believed that the use of LiF for this investigation does not restrict the significance of the 1 results. In fact, it is believed that this complements and extends previous papers by the same author which dealt with metal crystals.10,14 The dislocations were detected by means of the etching techniques that were described in a previous paper by Gilman and Johnston.3 In that paper it

Jan 1, 1958

By R. R. Spencer, C. A. Campbell, R. J. Marcotte, A. S. Kromer, P. H. Ostlender

Calumet Div. of Calumet & Hecla Inc. is engaged primarily in mining, milling, and smelting the native copper ores of northern Michigan. The copper occurs in fragmental tops of lava flows and in certain interbedded felsitic conglomerates of Pre- Cambrian age. The most famous native copper ore- body in world history is the Calumet conglomerate, which outcrops between the villages of Calumet and Laurium for a distance of about 2 miles. The Osceola lode parallels the conglomerate lode and is mineralized for about 3 miles. Horizontal distance between the two is 750 ft. In 1932 the price of copper dropped to 54 per lb. Coupled with the high cost of obtaining copper from extreme depths, this low price made the venture un- profitable, and the mining unit was abandoned. After the shaft pillar copper was removed from several of the conglomerate shafts in a retreating operation, the mine was allowed to fill with water. In post-depression years, when the price of copper stabilized at about 12¢, Calumet Div. found it profitable to operate its remaining mines on other lodes, as well as its tailings reclamation plants.

Apr 1, 1956

By J. Brian Eby

Contact metamorphism of coals is any physical or chemical change in the character of a coal directly attributable to heat of surface or intrusive igneous rocks. Coal beds so affected are found in the United States, England, Alaska, Mexico, New Zealand, Greenland, and other countries. Particularly in the United States, there is a wide occurrence of contact altered coals; conspicuous examples are found in Colorado, Utah, New Mexico, Illinois, and North Carolina. During a recent examination of coal beds on Yampa River, in northwestern Colorado, the author had an opportunity to make some detailed observations on the contact metamorphism of coals. In this field, coals over an area of 20 sq. mi. have been affected by dikes, sheets, and sills;' samples of the coals were systematically collected and analyzed,2 with the view of obtaining more specific data on the character of these alterations. The investigation was threefold in purpose: to secure information on the lateral effects of a dike cutting a coal bed, on the range in vertical effects on coal beds overlying sheets or sills, and on the range in the vertical effects on coal beds underlying sheets and sills. Favorable field conditions, such as fresh outcrops and newly dug prospects, made possible many of the field observations and collections. The coals studied in this field belong chiefly to the Mesaverde and 11Laramie" formations. The Mesaverde coals, on the average, are blocky low-rank bituminous coals; the "Laramie" coals, which are considerably younger, are of subbituminous rank. The coals of both formations, in the northeastern part of the Yampa field, have been greatly affected by basalt intrusives, yielding all variations of carbonized coal from natural coke to the unaffected material. The igneous rock that directly affects the coals is a fine-grained olivine basalt that is intruded, in sheets up to 200 ft. thick, into the coal-bearing

Jan 1, 1925

By T. A. Read, M. S. Wechsler, D. S. Lieberman

IN the formation of martensite in steel, it has been observed that the habit plane does not change continuously as the alloy content is varied. Instead, it appears that discrete habits correspond to certain ranges of composition. Greninger and Troiano' found that in low-, medium-, and high-carbon steels, the habits are approximately (1l1), (225), and (259), respectively.* The work of Mehl and Van Winkle2 indicated that the change from the (225) to the (259) habit is fundamentally a consequence of the lower transformation temperature rather than the higher carbon content. Also, Otte and Read3 observed that the habit plane orientation for a chrome-carbon steel scattered within a cone of semivertex angle of 5 deg, which was outside of the experimental error in the determination of the habit plane. These observations suggest the importance of investigating what factors in the crystallography of the formation of martensite account for the several types of habit and the inherent scatter in the precise orientation of the habit plane. A theoretical treatment of the austenite-martensite transformation has been given,4 which considers the total transformation distortion to be composed

Jan 1, 1961

By A. W. Ruff

In the last ten years large gains have been made in the field of blasting. These gains have been both in the theoretical and in the practical application of explosives. One of the most publicized changes in the practical application of commercial explosives is the now-prevalent use of ammonium nitrate and fuel oil. The new water-compatible mixture of ammonium nitrate and TNT should also have a large field of application. Most of the theoretical gains have been concerned with the actual rock breakage obtained with explosives. In the last ten years, large gains have been made in the field of blasting. These gains have been both in the theoretical and in the practical application of explosives. One of the most publicized changes in the practical application of commercial explosives is the now prevalent use of ammonium nitrate and fuel oil. The new water-compatible mixture of ammonium nitrate and TNT should also have a large field of application. Most of the theoretical gains have been concerned with the actual rock breakage obtained with explosives. EXPANDING-GAS-BUBBLE THEORY There has been an outstanding change in the conception of how an explosive produces rock failure. The early theory which explained rock breakage was correct for some of the first force-producing agents such as quicklime. When a drillhole was filled with quicklime and water added, the material expanded and steam was generated. The expanding material and the steam exerted a slowly increasing pressure on the sides of the drillhole. The force broke the rock by splitting. Because a great quantity of gas was produced by the deflagration of gunpowder, the same process of the gas pressure splitting the rock was assumed to take place. Even after 80 years of use, the rock-breaking action of all high explosives was thought to be caused entirely by the expanding gas bubble which tore and split the rock. Fig. 1 shows a vertical section through an exploding spherical charge of high explosive. It illustrates the early theory which attributed the entire breakage to the expanding gas bubble. The basic idea of this theory is that the breakage started at the explosive charge and progressed toward the free face. REFLECTED-WAVE THEORY me expanding-gas- bubble theory has gradually been replaced by the reflected-wave theory. The reflected-wave theory explains rock failure by explosives in the following manner: The enormously high gas pressure in the drillhole produces fracturing of the rock on the sides of the drillhole. The fracturing around a 1 1/2-in. diam drillhole is usually confined to an area with about a 6-in. diam. In the fractured area, the pressure of the gas is reduced until the force on the walls is no longer capable of fracturing the rock. Although the gas pressure does not continue to fracture the rock, the pressure imposes a high impact stress on the wall rock. In addition, a pressure or seismic pulse is produced in the rock. The pulse is probably entirely a compression pulse when originally produced in the rock. But, with distance, part of the energy of the compression pulse is transformed into a tension pulse which follows the compression pulse. The explosive charges and burdens used in conventional mine blasting are such that the tension pulse of the original wave is probably too small to be considered in a practical evaluation of the theory. The compression pulse is transmitted through the rock with no associated fracturing.

Jan 1, 1961

By H. W. Knott, M. H. Mueller

The crystal structures of Ti2Cu, Ti2Ni, Ti4Ni2O, and Ti4Cu20 have been determined using powder specimens examined by X-ray and neutron diffraction. Lattice constants have been determined for all four phases using X-ray powder diffraction films. Atom positional parameters of all four phases have been determined from observed neutron intensities. X-ray diffraction calculated intensity data have been presented also for the phase Ti2Cu to point out the particular suitability of neutron diffraction in this case. Interatomic distances have been determined using the positional parameters obtained from neutron diffraction. ALTHOUGH some investigations of the crystal structures have been made of these four compounds previously,'-13 it was the purpose of the present investigation to expand the previous work in order to locate the various atoms, determine their coordinates, and to confirm or to correct some of the previous work. It was convenient to group these four compounds together since they are related chemicallv and/or structurally. The compound Ti2Cu is tetragonil; and Ti2Ni, Ti4Ni2O, and Ti4CU2O are all large fees of the same space group. Ti2Cu has been previously reported as a fee phase by Laves and Wallbaum;1 and Rostoker2 which was possibly the oxide phase, Ti4Cu20. Joukainen, Grant, and Floe;3 and Trzebiatowski, Berak, and Ramotow-ski4 have also reported a phase of this composition. karlsson5 has reported a small fct phase of the composition Ti3Cu which may be the presently discussed Ti2Cu phase. More recently Ence and Margolin6 have reported a small fct phase for Ti2Cu and the present authors7 together with Nevitt8 have briefly reported it to be a bet related to the fct with a co three times the length of the co of the fct and have also reported that this phase has a very limited composition. Further refinements will be reported which have varied some of the parameters of this bct structure slightly. Ti2Ni has been reported as a fee phase by Laves and wallbaum;1 Duwez and taylor;9 Rostoker;2 Poole and Hume-Rothery;10 and Yurko, Barton, and parr.11 In a later paper Yurko, Barton, and parr12 have given the complete structure of this phase based on an X-ray diffraction study which was independently confirmed with neutron diffraction by Mueller and knott.7 Additional crystal structure information will be given. Ti4Ti2O, Ti4Cu2O, and a number of other compounds including Ti4Fe2O have been reported as fcc phases by Rostoker,2 and more recently Nevitt13 has confirmed the Ti4Ti2O phase. Rostoker,2 however has reported diffraction lines for Ti4Fe2O which do not have all odd or all even indices. These lines, therefore, cannot be observed if this compound has a fee structure. This same error has crept into the diffraction results reported for TiNi2O and Ti4Cu20 in the ASTM powder data which has been credited from Rostoker's data. Complete crystal structures of these two phases will be presented. Although all four of these structures have large unit cells and hence do not lend themselves for completely resolved neutron powder patterns, a sufficient number of individual reflections was observed for solving the structure. They also serve as good examples of some of the advantages to be gained by using both neutron and X-ray diffraction techniques. EXPERIMENTAL PROCEDURE All of the alloys were prepared by arc melting. The starting metals had the following purity: Cu 99.999 pct, Ni 99.83 pct, and Ti 99.92 pct. Oxygen was introduced into the two oxide phases as chemically pure TiO2, with the remainder of the titanium coming from the above mentioned metal. All of the sample buttons were annealed in evacuated Vycor tubes, the two binary phases for 5 days at 700°C and the two oxide phases for 3 days at 900°C. Oxygen analyses were performed on all four phases by two independent laboratories with the following amounts of oxygen present in atomic percent; Ti2Cu-0.06, Ti2Ni-1.03, Ti4Ni2O-13.95, and Ti4Cu20-13.87. The stoichiometric amount for the oxide phases is 14.29 at. pct. Since all of the samples were very brittle they were easily reduced to a powder for diffraction measurements. The lattice constants given in Table I were determined for the four compounds from X-ray diffraction patterns of powder samples exposed to filtered copper radiation using a 114.59 mm diam Debye-Scherrer type camera using the Straumanis loading. None of the patterns showed a detectable amount of a second phase. The lattice constants were obtained from an IBM 704 computer program employing a least squares treatment with systematic correction terms as previously reported.14

Jan 1, 1963

By C. Baldwin Sawyer

J. S. Vanick,* Washington, D. C. (written discussion).—To those who have been confronted with the study of the gas-metal reactions, this paper is a most welcome contribution. My personal interest in work bearing upon this general problem, stimulated by an appreciation of the difficulties inherent to problems of this type, prompts a few words of discussion. Table 2 of the paper shows a gradual increase in the nitrogen content with an increase in pressure, and an interpretation follows in which nitrogcn is used as the compressed medium when the conditions admit that cyanogen gas could be active as a contaminating ingredient. Fusions of electrolytic iron made in the induction furnace in an atmosphere of deoxidized nitrogen and out of contact with contaminating materials have shown no microscopic evidence of -a nitrogen increase; using a refractory-lined graphite crucible in the furnace under the same conditions or admitting air often resulted in the occurrence of nitride needles in the solidified melt. These results suggested that a nitrogenous compound served as a vehicle for the introduction of nitrogen and that such compound was not available when the pure gas and carbon-free refractory were used. The fusion of pure iron in pure nitrogen is perhaps a matter of theoretical interest. The author's work serves a more practical purpose when applied to steels rather than iron. Table 2 reports the absence of nitride needles in melts made under pressure of one atmosphere, although the quantity of nitrogen present would seem to exceed microscopically detectable percentages. In some recent work29 on carburized iron, nitride needles have been observed in areas analyzing as low as 0.015 per cent. nitrogen. This low percentage of nitrogen would indicate that the solubility limit is less than 0.030 per cent. for hypoeutectoid steels. There is the possibility that the areas of pearlite which exist in a hypoeutectoid steel restrict the distribution of nitrogen and limit its presence to the ferritie fields. In view of this work and the references quoted by the author, I am led to expect that the value for the solubility of nitrogen in solidified iron may approach

Jan 1, 1924

By Frank H. Macpherson

When it became apparent early in 1941 that the United States might be drawn into the war, studies were made of the bauxite situation in Arkansas, principally because 9.5 pct of the known bauxite reserves of the country were located in that State. Bauxite mining was then geared for maximum production to supply ore to meet this country's war requirements and, if necessary, to supply the needs of Canada as well. In view of the comparatively small bauxite reserves, Congress appropriated funds for an extensive exploratory drilling program to be carried out by the Bureau of Mines in cooperation with the Geological Survey. An alumina plant was erected near Bauxite and an aluminum plant near Hot Springs, Ark., by the Defence Plant Corp. The Metals Reserve Co. established a schedule of prices, arranged for stockpile sites and a buying agency. Operators cooperated to step up production and new ones came into the field. Production Record Prior to 1941, the greatest annual production in Arkansas was 562,892 long tons, dry basis in 1918. During the single month of August 1943, 693,596 long tons were mined—130,704 tons more than for the entire year of 1918. In general the Arkansas bauxite deposits are relatively small, irregular in thickness, somewhat scattered and, compared to coal, iron or open-pit copper deposits, are ill-adapted to an expansion in output. Commercial deposits range in horizontal extent from less than an acre to about 40 acres and are usually very irregular in outline. The average thickness of all known workable deposits is between 12 and 15 ft. with a maximum of about 60 ft. The ore bodies are usually somewhat undulating and nearly horizontal although locally some deposits dip as much as IS°. Types of Bauxite Three physical types of bauxite may be recognized: pisolitic, granitic and amorphous. Pisolitic ore is the most common type. It consists of small pebble-like nodules, ranging from the size of a pin head up to several inches in diameter, all set in a fine grained matrix. Transported bauxite is usually- pisolitic. Most residual bauxite is granitic. It is believed not to have moved appreciably from the location where it originally was formed. This is indicated by the fact that it appears to grade into unaltered nephelite syenite, which it overlies. Amorphous ore is the least abundant. It is nonpisolitic and resembles clay, has no characteristic texture, and can be identified definitely only by chemical analysis. Uses of Bauxite Bauxite is chiefly used for, and at the present time is substantially the only

Jan 1, 1948

By Frank H. Macpherson

When it became apparent early in 1941 that the United States might be drawn into the war, studies were made of the bauxite situation in Arkansas, principally because 9.5 pct of the known bauxite reserves of the country were located in that State. Bauxite mining was then geared for maximum production to supply ore to meet this country's war requirements and, if necessary, to supply the needs of Canada as well. In view of the comparatively small bauxite reserves, Congress appropriated funds for an extensive exploratory drilling program to be carried out by the Bureau of Mines in cooperation with the Geological Survey. An alumina plant was erected near Bauxite and an aluminum plant near Hot Springs, Ark., by the Defence Plant Corp. The Metals Reserve Co. established a schedule of prices, arranged for stockpile sites and a buying agency. Operators cooperated to step up production and new ones came into the field. Production Record Prior to 1941, the greatest annual production in Arkansas was 562,892 long tons, dry basis in 1918. During the single month of August 1943, 693,596 long tons were mined—130,704 tons more than for the entire year of 1918. In general the Arkansas bauxite deposits are relatively small, irregular in thickness, somewhat scattered and, compared to coal, iron or open-pit copper deposits, are ill-adapted to an expansion in output. Commercial deposits range in horizontal extent from less than an acre to about 40 acres and are usually very irregular in outline. The average thickness of all known workable deposits is between 12 and 15 ft. with a maximum of about 60 ft. The ore bodies are usually somewhat undulating and nearly horizontal although locally some deposits dip as much as IS°. Types of Bauxite Three physical types of bauxite may be recognized: pisolitic, granitic and amorphous. Pisolitic ore is the most common type. It consists of small pebble-like nodules, ranging from the size of a pin head up to several inches in diameter, all set in a fine grained matrix. Transported bauxite is usually- pisolitic. Most residual bauxite is granitic. It is believed not to have moved appreciably from the location where it originally was formed. This is indicated by the fact that it appears to grade into unaltered nephelite syenite, which it overlies. Amorphous ore is the least abundant. It is nonpisolitic and resembles clay, has no characteristic texture, and can be identified definitely only by chemical analysis. Uses of Bauxite Bauxite is chiefly used for, and at the present time is substantially the only

Jan 1, 1948

By J. Weertman

High-temperature creep experiments were carried out on indium, lead, and on binary substitutional alloys of In-Pb, In-Sn, In-TI, In-Cd, In-Hg, Pb-Bi, Pb-Sn, Pb-In, and Pb-Cd. The stress at which the power law creep equution breaks down was found to be much smaller for indium and lead than for metals with larger elastic moduli. The exponent over the stress in the power law creep equation was found to decrease upon alloying from values close to 4.5 to values near 3. THIS paper describes a set of high-temperature creep experiments made on high-purity lead and indium and on lead-rich and indium-rich single-phase binary alloys of various metals. These ex- periments were carried out to check two predictions of some creep equations derived by us"2 from a dislocation creep model due essentially to Mott. This model is shown in Fig. 1. Here dislocation loops are emitted from sources, not shown, situated on different slip planes. As the loops expand they come into each others' stress fields and are stopped. However, at high temperatures, as Mott has pointed out.

Jan 1, 1961

By H. Carroll Weed

By caving a block into the workings of its open pit and using the block as an ore transfer, the lnspiration Consolidated Copper Co. has solved a transportation and sizing problem, making possible a great expansion of open-pit methods as applied to Inspiration ore-bodies. FROM 1915 to 1948 the entire production of Inspiration Consolidated Copper Co. was supplied from underground mining. The sole method used was block caving. Underground haulage and hoisting facilities were designed and geared to large-scale production. Beginning in 1948 open-pit mining was substituted for block caving in a portion of Inspiration's Live Oak orebody. The idea proved so attractive that before the Live Oak pit had come into production, another pit on the Colorado orebody (now the Thornton pit) had been laid out and stripping started. It should be noted that these orebodies were not new and the entire program was one of changed methods of mining. Since part of these orebodies had already been mined by block caving methods, it must be recognized that haulage levels had been established under the area or adjacent to it. The orebodies lay on the south side of Inspiration Ridge, while the shafts, crushers, and treatment plants are all on the north side of this ridge. The existing main crushing plant was designed to take a maximum of 12-in. material, and all ore was sized to this dimension by passing through grizzlies in the stopes. In the original planning for open-pit work much thought was given to the transfer of ore to existing underground levels for haulage and hoisting from the regular shafts. If this could be done the necessity of crossing the ridge could be eliminated. Final decision called for cutting a road through the ridge, installation of a primary crusher at an elevation of 3968 ft on the north side of the ridge, and railroad haulage with existing facilities to the main coarse crusher. This decision was brought about by the difficulties of properly sizing and transferring to underground haulage large tonnages of coarse breaking oxide which lay on the upper benches of the proposed pit. Trucking over the ridge on a 7 pct grade would give a cheaper and more flexible operation in handling this material. The benches in the pits are laid out at 50-ft inter-vals and designated according to elevation above sea level. The lowest bench in the original pit was laid out at 3500-ft elvation. All haulage roads are on a 7 pct grade and a vertical lift of 468 ft was considered about the maximum economically possible from a cost standpoint. After 2 years' operation the advantages of pit mining, both from the standpoint of costs and flexibility of operation, became more and more apparent. Studies were then started to develop the extension of open-pit mining to more of the ore reserve than had been planned originally. The idea of transfer raises was again explored. Obviously, as elevation of the pit was lowered, shorter transfer raises would be needed to reach the main haulage levels. Transportation from the lower elevations to the rim of the pit by belt conveyor or skip hoisting was also considered. However, it was recognized that sizing would be required both for conveying and regulation of feed size to the main crusher plant. This would necessitate a fixed or portable crusher located somewhere in the pit. It was known that the sulphide ore at the lower elevations was softer and easier to break than the overlying oxide of the upper benches. This sulphide ore is very suitable for grizzly sizing. Calculations indicated that for ore mined on 3650 elevation, costs for trucking to the primary crusher, crushing, and delivery by railroad to the coarse crusher would equal costs for dropping the same material to the 600 level, hauling underground, and hoisting directly to the coarse crusher bins, provided a suitable method of sizing and transferring could be developed. Above 3650 elevation costs would favor surface haulage; below they would favor underground haulage. The idea of caving an underground block from the 600 haulage level directly into the bottom of the pit

Jan 1, 1954