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By C. C. Clark, J. S. Iwanski

The purpose of this investigation was to study mi-crostructural changes that take place in a commercial nickel-chromium-iron alloy, such as Incoloy "901," over long periods of time at temperatures up to 13 50°F and to correlate such changes with creep-rupture properties. of the alloy. In the course of the investigation, some microstructural changes were observed which correspond to microstructural alterations found in previous studies of Inconel "X." Microstructural phases have been identified in both alloys with the aid of electron and X-ray diffraction and an electron probe microanalyzer. The materials used in this investigation were from commercial heats of the following chemical composition: Pct Cr Pct Ni Pct Mo Pct Fe Pct Cb Incoloy "901" 12.51 43.67 5.72 Bal. -Inconel "X" 14.61 73.44 - 6.61 1.02 Pct A1 Pct Ti Pct Mn Pct Si Pct C Incoloy "901" 0.10 2.46 0.46 0.24 0.05 Inconel "X" 0.70 2.43 0.51 0.36 0.04 Long-term creep-rupture tests were conducted on Incoloy "901" at temperatures of 1000°, 1200°1 and 1350°F. A summary of these results is shown in Table I along with the results of a long-term creep-rupture test conducted on Inconel "X" at 1500°F. The heat treatments given the specimens are also shown in Table I. When the creep-rupture results on Incoloy "901" are compared with shorter-tertn data, there is no evidence of any undue deterioration of the creep-rupture strength with time, nor is the elongation decreased more than would be expected from the influence of time alone. INCOLOY "901" PHASE IDENTIFICATION Microscopic examination of the Incoloy "901" specimens reveals a dark etching grain boundary constituent in the specimen which was under test for about 11,500 hr at 1000°F. This grain boundary constituent was seen to increase in size as the test temperature was increased to 1200" and 1350°F, Figs. 1, 2, and 3. Simultaneously, an acicular structure of definite crystallographic orientation appears within the grains of the 1350°F specimen, Fig. 3. Under examination with the electron microscope, a fine precipitate is observed in the 1200 °F specimen. Fig. 4. It becomes considerably larger in the 2850-hr 1350°F specimen, Fig. 5. In a few areas the precipitated particles have been replaced by, or transformed to, small needles or platelets. After 7380 hr at 1350°F, Figs. 3 and 6, the needles are much larger and have replaced nearly all of the fine precipitate. X-ray diffraction studies detected the presence of hexagonal Laves phase and hexagonal n phase (Ni,Ti) in the 1350°F specimens, Table 11. Only the Laves phase was detected by X-ray diffraction in the 1200°F specimen and none was detected in the 1000°F specimen. In this latter specimen, however, the small quantity of precipitate in the grain boundaries (presumed to be Laves phase) precludes its detection by X-ray diffraction. Composition of the hexagonal Laves phase is not yet known, although its diffraction

Jan 1, 1960

By V. N. Mackiw

IN the process employed by Sherritt Gordon Mines Ltd. for the production of metallic nickel, a sul-fide concentrate is leached with ammonia and air under pressure. Following the removal of iron, copper, and other impurities, there remains a purified solution having the following analysis: 40 to 50 g per liter Ni, 200 to 400 g per liter (NH4)2 SO 4, and 20 to 30 g per liter NH3. Metallic nickel is reduced from this solution by hydrogen under pressure at 300' to 350°F in mechanically agitated autoclaves. A catalyst, ferrous sulfate, is required to initiate the first reduction. After the reduction, the depleted solution is discharged, leaving the metallic nickel in the autoclave. The nickel produced, being in a finely divided form, is used as a catalyst for the reduction of the next batch of solution. Upon repeated use the metallic nickel particles increase in size and become more compact, resulting in the production of a powder with higher apparent density. For this reason, each reduction is termed densification. Finally, when the burden of metal powder in the autoclave becomes too great to obtain effective agitation, both powder and depleted solution are discharged. The autoclave is then filled with fresh solution, ferrous sulfate catalyst added as before, and a new cycle started. The operation is described in earlier publications.1-6 A comprehensive historical review of the reduction of metals from solutions in general was given in a paper by Schaufelberger.7 The experimental data presented in this paper were taken from the work done in the Research Laboratory of Sherritt Gordon Mines Ltd. in Ottawa during the development of the process in 1951 and 1952. The results of the work were tested on a pilot plant scale in Ottawa in the period 1952 to 1953. Following laboratory and the pilot plant studies a commercial process has operated successfully since 1954 in the Nickel Refinery of Sherritt Gordon Mines Ltd. in Fort Saskatchewan, Alberta. General Experimental Technique The experiments were carried out in a stainless steel, 1-gallon, agitated autoclave designed and manufactured by Autoclave Engineers Inc. The inside dimensions of the vessel were 5 in. diam and 12 in. depth. The stirrer consisted of a 1/2 in. diam shaft 11 in. long fitted, with an axial flow type impeller (three blades bent to throw downwards) and a radial flow

Jan 1, 1958

By J. B. Clark, A. S. Yue

The zone-melting technique can be adapted for the de-termination of the eutectic composition in complex metal systerrzs. The application of this method is demonstrated in a simple eutectic system, Mg-AE, in which the eutectic composition is known and in a complex ternary system, Mg-Al-Zn, in which the literature is uncertain as to the composition of the ternary eutectic. The advantages and limitations of this unique approach for the determirution of the eutectic composition are discussed. ThE eutectic composition in phase diagrams is usually determined by thermal analysis of a series of arbitarily selected alloy compositions. The temperatures of the liquidus and eutectic arrests for each alloy are plotted and the eutectic composition is estimated by extrapolation to the entectic temperature of the curve formed by the liquidus arrest temperatures for the series of alloys. Although this approach readily yields the eutectic temperatures, several dekrminations are needed to estimate the eutectic composition, even in a simple system. In a complex ternary system, a great many determinations are often necessary to estimate, even approximately, the ternary eutectic composition. Thus, the conventional method is inherently tedious and time consuming. The application of zone melting provides a relatively efficient method of determining the eutectic composition.' As an illustration, consider the zone melting of an alloy composition C, in the simple eutectic system A-B, shown in Fig. 1, under the ideal conditions of infinitely rapid diffusion in the liquid, no diffusion in the solid, and ease of nucleation of both phases. As the zone moves along the bar, the composition of the zone is enriched by solute rejected during the freezing of the a phase and the zone composition approaches the eutectic composition CE.Once the zone composition attains the lowest melting composition, i.e., the eutectic composition, it remains at this composition as the zone moves along the bar and finally freezes as such at the end of the bar. Chemical analysis of the end of such a zone-melted bar then should yield the eutectic composition CE of the system A-B. A corresponding analysis can be made for a ternary eutectic system. Under the ideal conditions noted above, only one pass of the molten zone is required to yield the eutectic composition. Experimentally, however, a solute-rich layer forms at the solid-liquid interface2 and the composition of the zone does not attain the eutectic composition as rapidly or as uniformly as in the ideal case outlined above. But with agitation of the melt, the ideal conditions can be approximated experimentally. Also, as shown below, zone melting permits a cumulative build-up of the solute at the end of the bar to the eutectic composition. The purpose of this paper is to demonstrate this unique method for determining the eutectic composition. The method is here applied to two systems: first, to the binary Mg-A1 system, in which the composition is well established, and second, to the complex Mg-Al-Zn system in which there is doubt concerning the composition of the ternary eutectic. EXPERIMENTAL PROCEDURE The zone-melting apparatus used in this study is described in detail elsewhere.3 Briefly, the binary alloy rods (5/8 in. in diam and 9 in. long) and the ternary alloy rods (5/8 in. in diam and 6 in. long), with the compositions given in Table I, were zone

Jan 1, 1962

ANY discussion of State-supported schools of mining and metallurgy needs to be prefaced by a definition, since the first school to offer a mining curriculum, the Pennsylvania. Polytechnic College, was established by a grant from the State. But, so far as can be determined, it received no further State support. It would be tiresome to go into precise details, and it will be enough to stipulate that by State schools are meant those which derive their main financial support from regular appropriations made by a State legislature. The University of Michigan was the first of these to. offer a mineral industry curriculum; its story, as well as those of Wisconsin and Illinois, has been related in the preceding chapter.* Arranging the others in chronological order involves making a decision as to what weight to attach to plans for giving instruction, as contrasted with its effective initiation. This may appropriately be illustrated by the history of mineral industry education in California. CALIFORNIA Among those who came to California in 1849 and the following years were many New Englanders who had a keen interest in education. Some of them, mostly Congregationalists and Presbyterians, sought to establish a school of higher education around San Francisco Bay and eventually succeeded in opening the "Scientific and Classical School at Contra Costa" in Oakland, at Broadway and 5th St., on June 90, 1853. This prospered so well that it was chartered by the State as the College of California" on April, 13, 1855. Developing so rapidly that its quarters became. cramped, in 1864 it not only bought a tract of

Jan 1, 1941

By Norman C. Britz, Mortimer P. Buck

THIS PAPER DEALS WITH the practices used at the Huntington, Nest Virginia works of The International Nickel Company, Inc., in hot and cold rolling nickel and high-nickel alloys. The practical metallurgical aspects are discussed and a brief description of equipment given. The alloys covered may he divided into three main groups. based on their major constituents: 1. Nickel alloys, 2. Nickel-copper alloys. 3. Nickel-chromium alloys. The nominal compositions of the various alloys which are produced in most common mill forms are given in Table 1. Nickel, a commercially pure grade of nickel containing about 0.05 pct carbon as' the chief alloying element, is produced in all common Mill forms. "L" Nickel is commercially pure nickel in which the carbon content is held as low as possible, usually less than 0.01 pct. This grade of nickel is used chiefly for spinning and for special high temperature applications where its low carbon content enhances its corrosion resistance. "D" Nickel contains 4.5 pct manganese to provide improved resistance to sulphur embrittlement at elevated temperatures. "Z" Nickel is an age hardening grade of nickel containing carbon, aluminum, and silicon as the age hardening elements. This alloy combines the cor-

Jan 1, 1948

By M. H. Gaskell, D. M. Kehn, G. T. Pyndus

A correlation of the bubble point pressure for black oil systems is developed using the standard physical-chemical equations of soiutions. The correlation is based on 158 experimentally measured bubble point pressures of 137 independent systems and is expressed in terins of the usually measured field pnrameters— flash separation gm-oil ratio, rank oil gravity, total gas gravity, and reservoir temperature. The data were obtained on systems produced in Canada, Western and Mid-Continent01 United States, and South America. The average error (algebraic) in the representation is 3.8 per cent, and the maximum error encountered is 14.7 per cent. INTRODUCTION In the absence of experimentally measured properties of reservoir fluids, it is often necessary for the field engineer to make estimates regarding the fluid properties based on the usually measured producing parameters. To aid in these estimations, various correlations have appeared in the literature in recent years. Among the pertinent properties of interest is the bubble point pressure. A correlation for this parameter has been reported by Standing'. However, this correlation was based essentially on California produced crudes and this limitation was pointed out with its presentation. The correlation presented in this paper utilized data on crude oil systems from Canada, Wes- tern and Mid-Continental United States, and South America. CORRELATION DEVELOPMENT The basic assumption used in this development is the same as employed by Standing', There is a wide variety of ways to combine these parameters; however, in this instance the combination was made on the basis of Henry's law2. Accordingly, the relationship proposed is Although Eq. 2 defines an individual system, it is of limited value since H' is a function of gas-phase composition and the system temperature. It was observed that for the systems where the bubble point was measured at several temperatures that the ratio of the bubble point pressures and the ratio of the corresponding absolute temperatures (R) were practically identical. Thus, for correlation purposes the bubble point pressure may be taken as a direct function of the absolute temperature. This relation is valid only for those systems that are not near the critical point. Accordingly, this correlation will be inadequate for systems in the region of the critical point. The solubility of the various hydrocarbons found in the gas phase increases with the molecular weight. Thus, the saturation pressure should be inversely related to the gas gravity. Applying these principles to Eq. 2 and rearranging terms gives: The variables 02 the left side of Eq. 3 were designated as the "hubble point pressure factor". The number of mols of tank oil per barrel is a function of the "mclecular weight" of the tank oil. Although the tank oil is a complex mixture, it was assumed for the purposes of this correlation that a unique molecular weight could be assigned to a given oil. This was designated as the "effective molecular weight", and was related to the oil gravity, This empirical relationship was developed simultaneously with the correlation by assuming values of M,. and working to obtain a smooth curve for both the correlation and the effective molecular weight. The relationship between the oil gravity and the effective molecular weight used in this correlation is shown in Fig. 1. The effective molecular weight is somewhat higher than the molecular weight of the C fraction. The difference between these values is largest for the low-gravity systems. It is noted that this effective molecular

By O. J. Huber, P. D. Frost, H. A. Robinson

URANIUM is a (ß-stabilizing, eutectoid-forming element when alloyed with titanium. Udy and Boulger1 have reported that an alloy of 48.6 pet uranium in titanium retains ß-phase when quenched from the ß-region, while compositions of approximately 30 pet uranium transform to martensite during such quenching. Since the eutectoid reaction is rather sluggish, titanium-uranium alloys should be capable of being strengthened by the ß — a trans-

Jan 1, 1959

By H. R. Froning, R. O. Leach

In wertability alteration flooding, a chemical agent is rnoved through a reservoir by the flood water to increase oil recovery by decreasing the degree of wetting of the rock by the oil. Substantial amounts of the chemical may be lost during movement through the reservoir. The extent of the loss, and therefore the economics of the process, depends in some cases on factors which are difficult to reproduce in the laboratory. Therefore, a short-duration, low-cost field test method is needed to permit evaluation of chemical requirements under actual field conditions. This paper describes a small scale rest conducted at a single well for measuring chemical requirements, thereby giving a more reliable evaluation of this important factor in the applicability and economics of the process. In the rest a small wafer slug containing the chemical agent and a nonadsorbed tracer is displaced into the reservoir by a known volume of wafer. The well is then placed on producrion. Chemical loss per barrel of pore volume contacted is calculated from [he fractional recoveries of the agent tested and the nonadsorbed tracer. The method has been used to determine within the actual reservoirs the chemical requirements for both a sandstone and a dolomite reservoir. Several chemical agents are potentially available for wettability alteration flooding, although none is universally applicable. For some applications of the method, chemical costs per barrel of additional oil recovered can be substantially less than one dollar. INTRODUCTION Wettability alteration flooding provides a means of increasing oil recovery from reservoirs by decreasing the degree of wetting of the rock by the oil and increasing the displacement efficiency of the flood water. Earlier studies demonstrated a relationship between oil recovery during waterflooding and the degree of wetting of a rock surface by an oil. The application of wettability alteration flooding to the Harrisburg field of Nebraska provided a field test' of this recovery process. Subsequently, additional laboratory and field tests have developed additional procedures for evaluating wettability alteration flooding, and have indicated where the process may be applicable. Applicability of this process to specific reservoirs is determined by a progression of tests to determine sus- ceptibility of the reservoir to alteration of its wettability, to indicate the degree of recovery improvement and to estimate the amount of chemical required to process the reservoir. The economics of applying improved oil recovery processes depends not only upon the degree of improvement in oil recovery achievable by the process but also upon the process costs and the timing of the income and the investment. Emphasis in this paper is on the expenditure aspects of the process. The work reported in this paper indicates that the chemical investments required for wettability alteration flooding are substantial. For evaluating the economics of a potential flooding application it is imperative that a sound estimate of the chemical requirements be made for the reservoir. Generally, true reservoir conditions are not adequately simulated in laboratory chemical propagation tests. Because of wide well spacings, many years might be required to obtain chemical propagation data from conventional pilots or inter-well tests. Consequently, n short-duration, low-cost method is needed to determine chemical requirements in the field. The potential applicability of wettability alteration flooding is discussed, as well as the economics of wettability alteration with respect to the inherent and imposed restrictions on the timing of income and investments. DETERMINATION OF CHEMICAL REQUIREMENTS In the process of moving a chemical bank through reservoir rock, some of the chemical agent lags too far behind the flood front to be effective or is otherwise lost to the reservoir system. The extent to which these losses occur overshadows the reductions in chemical concentration due to diffusion and to mixing with the reservoir fluids. Experience indicates that almost without exception, chemicals which induce a wetting change undergo either sorption reactions or chemical reactions with mineral constituents of the pore surfaces. Other reactions may occur between the added chemical and the reservoir oil and water. Even in limiting consideration to reactions of the relatively inexpensive inorganic salts, bases and acids, the reactions may be exceedingly complex. Reservoir pore surfaces consist of more than silica in sandstone reservoirs, and more than calcite or dolomite in carbonate reservoirs. Many mineral species are present, each exhibiting specific tendencies to react with an injected chemical. The reactions which occur can consume enough of the agent to have an important effect on economics. These reactions can cause a change in pH of the chemical bank, or may remove some of the active chemical by precipitation, adsorption or reaction to form a new chemical which may or may not be effective in

By W. A. Gibson, Zay Jeffries

It has been known for a number of years that certain aluminum alloys could be hardened by quenching from a temperature of about 500' C. Immediately after quenching the total increase in hardness is not marked, but the hardness increases gradually so that after about 4 days, it has reached a maximum. The actual increase in hardness probably continues for weeks or even months, but in order to detect the differences after 4 days, it is necessary to make tests at rather long intervals. So far as is known to the authors, Alfred Wilm was the first to discover these properties in aluminum alloys.' The aluminum-copper alloys are amenable to this treatment and the addition of magnesium makes the heat-treatment effect more pronounced. Until recently heat treatment of aluminum alloys has been confined to the worked alloys in the form of sheet or extruded products. The alloy that has been most used in this connection is known commercially as duralumin and has about the following composition: copper not exceeding, 6 per cent.; magnesium not exceeding, 2 per cent.; manganese not exceeding, 1 per cent.; commercial aluminum,2 balance. A typically good alloy in this range consists of: copper, 4 per cent.; magnesium, 0.5 per cent.; manganese, 1 per cent.; commercial aluminum, balance. This alloy can be rolled into sheets or extruded; and in this condition it can be heated in the ordinary furnace atmosphere to a temperature near 500° C. and quenched in water. After about 4 days it will have the following physical properties: tensile strength 55,000 to 60,000 1b. per sq. in. (3866 to 4218 kg. per sq. cm.); elongation in 2 in., 15 to 20 per cent. No harmful effects of the furnace gases or even the air, if the heating is effected in an electric furnace in an air atmospherc.

Jan 1, 1921

By Albert J. Phillips

When brasses containing from 61 to 62.5 per cent. copper are very rapidly cooled from temperatures near their melting point to below 0" C., unusual results are obtained. These results are quite unexplainable from a consideration of the old copper-zinc constitutional diagram but they can be satisfactorily explained by means of the diagram revised by Genders and Bailey1 (Fig. 1). Experiments on a 60/40 Brass If an alloy containing 60 per cent. copper is heated to any temperature between approximately 760' C. and its melting point, it will consist entirely of beta. Upon slowly cooling, alpha will start to separate just below 760" C. Since this alpha will contain nearly 65 per cent, copper, the beta will be impoverished by its separation. As the temperature decreases the composition of the separating alpha will approach approximately 61 per cent. and the beta in contact with the alpha will maintain an equilibrium composition approaching 54.5 per cent. copper. If the rate of cooling is extremely slow, especially at the lower temperatures, stable equilibrium will be established by diffusion through the alpha and beta so that eventually 85 per cent. of the alloy will consist of alpha containing 61 per cent. copper, while 15 per cent. will be beta containing 54.5 per cent. copper. With a faster cooling rate diffusion cannot keep apace and the constituents will be cored, the alpha varying from 65 to 61 per cent. copper and the beta from 60 to 54.5 copper. In this case the amount of alpha will be less than 85 per cent. and the beta will be increased correspondingly. The general structure thus obtained is illustrated in Fig. 2. When a more rapid rate of cooling is effected by quenching in water, the alloy is retained largely in the beta form. However, the crystals of beta are usually outlined with dark fringes which at high magnifications are found to be very fine alpha-beta structures almost martensitic in appearance. The separation of this fringe can be greatly suppressed

Jan 1, 1930

By A. A. Smith, J. S. Smart

THE elements silver, cadmium, tin, antimony and tellurium either are found as impurities in commercial coppers or are intentionally added to produce coppers for special uses, When present in small quantities, each of these metals exerts a significant effect on the properties of copper, but despite considerable experience and investigation much remains to be learned about their specific behavior. The presence of extraneous elements, particularly oxygen, complicates the study of individual additions of impurities in the range 0 to 0.05 per cent, and the use of high-purity copper has been found extremely helpful in circumventing these difficulties. It has also been found that individual behavior can be satisfactorily determined from measurements of two commercially important properties, conductivity and softening temperature, according to methods that have been described previously.1,2 Data of this type, obtained in the course of a general investigation of the effects of impurities on the properties of both oxygen-bearing and oxygen-free copper are presented herewith. All samples except those containing cadmium were prepared as 3/8-in. continuously cast oxygen-free rod from pure copper and weighed amounts of a similarly synthesized master alloy. Composition was checked by chemical methods, which in every case verified the calculated analyses. Test wires were cold-drawn one B. and S. number per pass on a string-up machine using four 30-min. 600°C. anneals at 0.3125, 0.257, 0.204 and 0.162 in. and a final cold reduction of 75 per cent to 0.081 in. Some oxygen-bearing samples were produced directly from the 3/8-in. oxygen-free rods by diffusion from a surface scale at 850°C. and drawn to size as listed above, but most of the alloys were remelted in pure graphite and cast through air into a I-in. round mold, The slugs were then hot-rolled to 5/16 in., drawn to 0.162 in., annealed as listed above, and drawn to 0.081 inch. Conductivity wires were annealed for I hr. at 100°C. intervals between 300° and 800°F., using a hydrogen atmosphere for oxygen-free samples and purified nitrogen for the oxygen-bearing type, All samples were quenched from the annealing temperature in 10 per cent H2SO4 and conductivity was measured on a Hoopes bridge that had been checked against a Kelvin bridge. The softening temperatures represent the half-hard stage of the annealing curve as determined by a standard procedure.1 EFFECT OF SILVER Numerous excellent studies of the argentiferous coppers are found in the literature, and these have been adequately

Jan 1, 1943

By H. R. MacMichael

THE rate, at which zinc ore can be sintered varies widely, depending on the characteristics- of the ore. A coarse table concentrate already roasted to a very, low sulfur content may sinter at the rate of-8.6 tons per hour per 100 sq.ft., of wind-box area. At the other extreme is a finely ground flotation, concentrate, with considerable sulfur remaining in the ore as delivered to the sinter plant, for which corresponding rate may be only 3.8 tons per hour, or 44 per cent of the first rate. A usual, size-of sinter machine in zinc plants is one with wind-box 3.5 by 33 ft., making 115.5 sq. ft. of area, and using a 100-hp. fan. Such a machine with the coarse concentrate described would produce 10 tons of sinter per hour; and with the fine, flotation concentrate would produce only 4.4 tons per hour. Ore of the latter class is -sintered at the plant of the Mexican Zinc Co. (subsidiary of the American Smelting & Refining Co.) at Rosita, Mexico. ; Consequently, an unusually large sintering capacity per ton of ore to be treated is required, and provision was made for treatment of 9000 tons concentrates per month, preroasted to. 5 to 9 per. cent sulfur. For this duty three of the usual 33-ft., 100-hp. sintering machines would have been needed.. Considering the auxiliary equipment. necessary for proportioning, handling, and mixing charge, as well as means for disposition of the sinter, a three-unit plant becomes-very complicated, especially if the capacity should be doubled later. After much study it was decided to build a single sintering unit of ample capacity for the work, the plant thus being much simpler and cheaper in construction as well as in operation (Figs. 1 and 2). The sintering machine was built with a wind-box 5.25 by 60 ft. (315 sq. ft.) and provided with a 300-hp. fan.

Jan 1, 1932

By John W. Cloud

IN 1877 the Pennsylvania Railroad Company removed an old bridge from its line at Duncannon, Pa., built intermediate piers and erected shorter spans of the Pratt truss type, which had previously been in use on another portion of the road. The design of this truss would not admit of diagonals larger than 1 5/8 inches diameter, and in order to stiffen the bridge somewhat steel rods were introduced for the main diagonals in the first and second panels, 1 5/8 inches and 1 3/8 inches diameter respectively. These rods were threaded without upsetting, and by the ordinary formulae the strains were of the same intensity upon both, viz., 16,000 pounds per square inch with the maximum loading. The other main diagonals in the truss are 1 5/8 inches diameter, and of iron. It was specified for the steel rods : Elastic limit, - 45,000 lbs. Tensile strength, - 80,000 lbs. Elongation, - 20 per cent. The steel was procured without difficulty, and it allowed a factor of safety of 2 3/4 at elastic limit, while a similar factor of 2 1/2 had for a long time been successfully used for iron. In the course of three years, from time to time, six of these steel rods broke, three of them being 1 3/8 inches in diameter, and three 1 5/8 inches in. diameter. The broken rods were tested, and three of them. analyzed at Altoona to ascertain the cause of failure, and what modi¬fications should be made in the steel for such service. Examination showed that all the rods were broken in detail close under the nut. The threads were well cut and properly rounded at the root. In testing the rods micrometer screws,. reading to .0001" with electric bell to signal the contact, were attached to the test pieces, and by this means the modulus of elasticity and elastic limit accurately obtained.

Jan 1, 1881

By Alexander L. Holley

THE 400-ton testing machine, ordered in June, 1875, by the United States Board appointed to test "iron, steel, and other metals," has lately been completed at the Watertown Arsenal, thoroughly proved and accepted by the Board. The excellence of the machine in every respect is more than satisfactory, and its accuracy is at first sight astonishing, although an investigation of its principles must show that if the weighing apparatus will weigh at all, it must do so with perfect accuracy, because all its movements are absolutely without friction. The proof experiments were numerous, and the effects of recoil after sudden ruptures at maximum loads, were watched with great care, but without much anxiety, because the weighing parts affected are by no means delicate in structure, and their motion is almost infinitely small. Among the tests were the following : A forged link of hard, wrought iron, 5 inches in diameter between the eyes, was slowly strained in tension, and broke short off with a loud report at 722,800 pounds. The diameter before breaking at the point of fracture was 5.04 inches; after breaking, 4.98 inches. In order to see if the weighing parts had been disturbed by the recoil, which was obviously near the greatest recoil the machine will ever suffer, a horse-hair was next tested ; it was 7-1000ths of an inch in diameter; it stretched 30 per cent., and broke at 1 pound. Other horse-hairs vary in tenacity between 1 and 2 pounds. Of course, the accuracy of the machine on such delicate specimens, and indeed on specimens having some hundreds of pounds tenacity, has been checked and proved by other weighing machines. A 5-inch round bar, turned down to 3 5/8 inches diameter along the centre, was pulled apart at 430,200 pounds tension. Then some more horse-hairs were tested ; also copper wires 19 1/2-1000ths of an inch in diameter, which averaged 25 pounds tenacity..

Jan 1, 1879

By Lyndon L. Foley

The proper spacing of oil wells is a problem of vital importance to the oil industry. Conservation demands a maximum recovery, while economic considerations attach primary importance to profitable extraction of oil. Formulas have been evolved,1-4 which attempt to solve the spacing problem mathematically, using reservoir characteristics as factors. Comparisons have been made of fields producing from supposedly similar sands, which have been drilled to varying densitiesl5,6 and also of different leases in the same field. 5-8 Intermediate wells have been drilled in old, depleted fields to test the efficiency of drainage by the original operation.9-11 Intermediate wells have been drilled also to obtain cores of the depleted sand for analysis, from which to learn the degree of efficiency of extraction. The problem is being attacked by many students, and along several different lines. Unfortunately, the fields now depleted were produced generally without restriction, and conclusions drawn from them may not apply to fields operated under restricted production. Reservoir conditions in a restricted field, especially reservoir pressures and pressure gradients within the reservoir, are quite different from those in a field produced to capacity. Many people have held the idea that the closer the spacing, the greater the recovery. This general statement is not always true, as other factors than well spacing enter into the recovery problem. Cutler,5 who has been quoted frequently by advocates of close spacing, limited his conclusions to gas-drive fields, and to the particular fields and spac-ings that he investigated. Hill and Sutton7 analyzed four tracts in the Powell field; the tract most closely drilled had the third largest recovery per acre-foot, and the tract with the widest spacing had the second largest recovery per acre-foot. A search of the references to well spacing in the publications of the U. S. Bureau of Mines5,13-19 discloses repeated condemnations of the wastefulness of the practice of town-lot drilling.

Jan 1, 1938

By Colin M. Sargent

THE electron diffraction pattern as seen in the electron microscope represents an approximately plane section of the reciprocal lattice. Identifying the zone axis of a diffraction pattern is often laborious for a crystal of low symmetry, especially if several crystal orientations are present. A program has been written in FORTRAN II (Version 2) for the IBM 1620 which will assist in plotting out reciprocal lattice sections. The calculation is performed by choosing a zone axis [uvw] and determining the d spacings and angle between the planes (Ow - v) and (wO - u). (This procedure is varied slightly for zone axes with Miller indices equal to zero.) Cartesian coordinates for the reciprocal lattice points are then calculated for these planes and for (ww— [u + v]). Any reciprocal lattice points within the parallelogram formed by the origin and these three points are then computed. The input and output are best described by use of an example (Monoclinic ZrO2) used in the author's work. Input consists of two cards: 1) The crystal parameters: a, b, c, a, 8, y, e.g., 5.1477, 5.2030, 5.3156, 90.000, 99.380, 90.000. 2) Three numbers, D, E, F, e.g., 5, 3, 3.0710-the first is the limit of the sum (u + v + w) considered; the second limits the absolute value of u, v, and w to (E- 1), e.g., 2, so that zones (221) would be the highest order considered in this example; the third, F, is the required constant, yL. Output is in the format shown in Table I. The reciprocal lattice sections may then be plotted on standard graph paper and compared with the unknown diffraction pattern. (Note that no attempt has been made to deal with systematically absent reflections.) A card deck for the program is available from Colin M. Sargent, ARZ, W-PAFB, Dayton, Ohio, 45433.

Jan 1, 1969

By E. Buehler, E. Berry

HE magnetic properties of dilute palladium alloys are of fundamental interest.''' Neutron diffraction studies3 have indicated that a better understanding of the behavior of these alloys could be realized with the availability of high-purity single crystals of palladium. Crucible melts of 99.999 pct pure palladium were found inadequate for such research. In a successful effort to fill this need, floating zone refining of palladium was undertaken. In this note the results of the initial experiments are reported. Zoning was accomplished in an argon atmosphere using 450 kc rf generator for an energy source. Samples 5 to 6 mm in diam were suspended in a gastight quartz envelope which could be moved vertically through the rf coil. A nominal upward traverse rate of 1.5 mm per min was maintained during a pass. Close coupling was found to be essential for stable retention of the liquid in the zone. Single crystals averaging 3.5 cm in length were obtained. Laue photography showed them to be continuous single crystals without gross imperfections. Several criteria were used for evaluation of the purity of the zoned material: magnetic behavior, low-temperature specific heat and residual resistivity ratios. Table I shows the residual resistance ratios obtained for two samples, one subjected to a single pass, the other zoned four times. It is appilrent that palladium can be zone refined with the electrically active impurities being transported toward the tail end. A decrease in susceptibility for zone-melted specimens over any previously measured material from 1.5" to 80'~ has been obserted by H. J. Williams and R. C. Sherwood4 substantiating the residual resistance data. The specific heat measurements are currently being made3 and will be published at some later date. Discussions with J. H. Wernick and S. C. Abrahams are acknowledged. We also wish to thank G. F. Brennert for the residual resistance measure ments.

Jan 1, 1962

By R. E. Reed-Hill, W. H. Hartt

High-purity magnesium single crystals, oriented with basal plane parallel to stress axis, were deformed in tension at room temperature so as to form second-order (1011)- (1012) twins. Investigation by optical and replica electron microscopy revealed that these twins can support very large internal strains approaching 1000 pct and that fracture follows as a direct consequence of these strains. At low strains the basal plane within (10i1)- (10i2) twins rotates with increasing deformation until it becomes approximately parallel to the twin boundaries. This rotation is not consistent with deformation by basal slip in the double twin, but may be rationalized in terms of nonbasal slip. Observations also indicate that basal slip in the primary (1011) twin, prior to second-order twinning, may contribute to this rotation. Deformation markings that are difficult to interpret in terms of slip on previously observed systems were noted in the twin bands. A possible means of rationalizing these markings is to relate them to grain boundary shear. The fracture associated with these twins is thought to initiate by formation of voids at the twin boundaries. These grow into microcracks, with ultimate fracture occurring by tearing of the interconnecting regions. THE significance of deformation and fracture along second-order (10i1)-(10i2) twins in polycrystalline magnesium1-' and many magnesium alloys4 was discussed in a previous paper.5 It was noted that this double twinning mode effectively controls the room-temperature deformation and fracture of magnesium single crystals, oriented with the basal plane parallel to the tensile axis. Reed-Hill and Robertson6 observed that, although these crystals may fracture at a macroscopic strain of less than 1 pct, shear strains up to 1000 pct could occur within (1011)- (10i2) twin bands. They concluded that the fracture was "ductile" and resulted from concentrating the deformation into a very small volume. The present research was undertaken to obtain a better understanding of the deformation and fracture associated with these twins. EXPERIMENTAL TECHNIQUES The experimental procedure involved straining high-purity magnesium single crystals in tension at room temperature. Specimens were oriented so that the applied stress direction was within 2 deg of the [1010] crystal axis. The specimen cross section was rectangular with faces closely parallel to (1210) and (0002). The specimen preparation and testing procedures have been described in detail elsewhere.5 Second-order (1011)- (1072) twins nucleated during straining were studied using optical and replica electron microscopy techniques. For the latter, cellulose acetate-carbon double replicas were employed. Observations were made on the (1210) crystal surface, which is the plane of shear for twins of this type. In addition to the single crystals, some investigations were carried out on longitudinal polycrystalline specimens. These were obtained from high-purity magnesium plate with a texture in which the basal planes of the grains tended to be nearly parallel to the specimen axis. All. polycrystalline specimens were annealed prior to testing in order to produce a coarse grain structure, permitting Laue back-reflection X-ray photographs to be obtained from grains of interest. EXPERIMENTAL RESULTS a) Deformation Within ( 101 l )-( 1072) Twins. Fig. 1 is an optical micrograph demonstrating the extent of the plastic deformation that can occur in (1011)-(10i2) twin bands. Notice at the lower left corner of the photograph the large displacement of the dark band (a polishing step) where it crosses the twins. The shear strain in the twin band at this position was computed to be 700 pct, using the ratio of step width to twin thickness. It was previously shown5 that (1011)- (1012) twin bands are often composed of small, separate twins aligned close to the macroscopic habit plane. Fig. 2 is an electron micrograph from near the upper end of the twin band in Fig. 1. This illustrates that the twin habit often does not coincide exactly with the macroscopic band habit, but may be inclined at a slightly smaller angle to the matrix basal plane. Figs. 3 through 6 are electron micrographs of the twin band in Fig. 2 illustrating successive steps in the development of deformation inside the band. A twin band such

Jan 1, 1969

By B. W. Levinger

THE system Ti-CI- has been studied by several investigators." ' Though titanium and chromium are completely miscible at high temperatures, an intermediate phase of the approximate atomic proportions TiCr, has been identified at various compositions between 60 and 68 wt pct Cr. The structure of this phase was established as the cubic C15 (MgCu2) type with 24 atoms per unit cell and a lattice parameter 6.929 kX.2 During a study of the ternary system, Ti-Mo-Cr,5 the existence of a high temperature modification of the TiCr, phase was discovered. In a series of alloys annealed at 1300°C and containing from 60 to 70 wt pct Cr and 5 pct Mo, a new phase was present which did not correspond to either ß solid solution or TiCr,. By trial, the new phase was identified to be of the hexagonal C14 (MgZn2) structure with 12 atoms per unit cell. Further work showed that the hexagonal structure was. in fact, also present in binary Ti-Cr alloys quenched from high temperatures. To make the identification more certain, the intensities of the various reflections were calculated assuming a composition TiCr2 and C14 structure. Table I lists reflection planes, interplanar distances, calculated intensities, and a comparison of these values with the lines of a binary Ti-Cr alloy (66 pct Cr) annealed for 20 min at 1385°C and water quenched. Since high angle lines were more diffuse, the correspondence between visually observed and calculated intensities was not as good at these angles. Lattice parameters were computed to be a = 4.922 kX, c = 7.945, c/a :- 1.614. The corresponding interatomic distances are: titanium to titanium distance, 3.00:, kx, chromium to chromium distance, 2.43, kX, titanium to chromium distance, 2.88,, kX. These compare to 3.00, 2.45, and 2.87 kX in the cubic phase, respectively.' The atomic positions in the C14 structure are as follows: Titanium 1/3, 2/3, Z; 1/3, 2/3, 1/2: 2/3, 1/3, i; 2/3, 1/3, (1/2-z); Chromium 0, 0, 0: 0, 0, 1/2; 2x, 2, 1/4; 232, x, %; X, 22, 1/4; X, 2x, 3/4; x. x, 1/4; x, x, 3/4; The values of x and z were calculated for the alloy mentioned and found as follows: z — 0.061, x = 0.165. The values assumed in the intensity calculations were those for an ideal close-packed lattice or z = 1/16, x = 1/6. Work in the Ti-Mo-Cr system indicates that y2 the hexagonal modification of TiCr2, is the stable phase above 1300°C, while y1 with the cubic structure is stable below 1000°C. X-ray examination of a number of alloys annealed at intermediate temperatures showed that the hexagonal and cubic phases can coexist. Alloys quenched from 1000°C and annealed at 1100" and 1200°C showed small amounts of y2 at the higher temperature. A considerable amount of y, seemed present, however, in cast alloys annealed at 1100°C. It further appears that there is a small but definite solubility range for both phases in the ternary system. Acknowledgment The results of this paper represent work carried out in conjunction with a project sponsored by Watertown Arsenal, Contract No. DA-11-022-ORD-272. References 'M. K. McQuillan: Journal Inst. Metals (1951) 79, p. 379. 2 P. Duwez and J. L. Taylor: Trans. ASM (1952) 44, p. 495. W. J. Van Thyne,. H.. D. Kessler, and M. Hansen: Trans. ASM (1952) 44, p. 974. 1 F. B. Cuff, N. J. Grant, and C. F. Floe: Trans. AIME (1952) 194, p. 848; Journal of Metals (August 1952). Unpublished Research, Armour Research Foundation. "H. J. Wallbaum: Ztsch. Krist. 103, p. 391.

Jan 1, 1954

By George J. Bancroft

At the New York meeting of the Institute, April, 1907, I presented a paper entitled, The Formation and Enrichment of Ore-Bearing Veins,' in which paper I advanced the following propositions: (1) That the majority of mineralized veins are the product of expiring vulcanism; (2) that most of these veins were primarily mineralized by comparatively rich solutions in comparatively short periods of time; (3) that the solutions gained their metal-values from a comparatively rich source; (4) that there is a bary-sphere containing large amounts of the useful metals; (5) that eruptions spring from various depths and bring various kinds of magmas towards the surface; and (6) that only those eruptions which disturb the barysphere and bring a magma rich in metals sufficiently near the surface to be leached by vein-making solutions are productive of valuable ore-deposits, other eruptions producing barren veins. Ore-deposits due to magmatic segregation were not included in this general survey. As a result of considerable further study I have modified my views in some respects, while in others I feel more sure than ever of the ground taken at that time. That ore-bodies are infrequent occurrences and born of extraordinary conditions I think is now generally accepted. The theory that persisted for a time—namely, that ore-bodies were formed by the ordinary ground-water, which consists of extremely dilute solutions, derived from leaching extremely lean surface-rocks, and which must occupy enormously long periods of time in concentrating the values so leached, is, I think, now pretty generally regarded as not applicable to the great majority

Jan 1, 1910