Search Documents

Doctor David Yang has presented an important new flotation development in the area of fine particle flotation technology; at the same time Dr. Yang presents an explanation for the effectiveness of this improved new fine flotation system in terms of an optimum dispersion state. The same statement is made for the case of carrier flotation (ultraflotation), in the removal of anatase from kaolinite by addition of calcite (selective flocculation of the anatase - calcite system and dispersion of kaolinite). Dr. Yang's data and statements raise some important questions, and I will adress myself to the more fundamental aspects of this new flotation system. The addition of sodium silicate, well known as a good depressant-dispersant agent for siliceous gangue minerals, is proved to be greatly enhanced by the incorporation of polyvalent metal salts into sodium silicate prior to flotation, producing in this manner a condition, as described by Dr. Yang, of optimum dispersion, which in the case of fine-grained oxidized taconite can be described as selective flocculation (coagulation) of hematite and almost complete dispersion of siliceous gangue components. Dr. Yang recognizes that the main mechanism, while not completely understood at this time, seems to operate by modifying the surface characteristics of the gangue slime particles so as to prevent collector from bonding there to, and making the particles strongly hydrophilic so they will become fully dispersed and consequently will not float during froth flotation. At the same time it appears that the conditioning reagent also modified the surface characteristics of the floated minerals (hematite and spodumene in this case) so that they will aggregate and tend to more readily adsorb the collector, resulting in an improved flotation kinetics and selectivity.

Jan 1, 1979

By Persifor Frazer

It was my intention to have directed the attention of the members of the Institute to a complete series of rocks representing the older and middle formations represented in Pennsylvania, but time has been insufficient for the purpose, and 1 have been unable, in the first attempts to reduce the sections of those rocks, which I have brought with me to this meeting, to the requisite thinness necessary for exhibiting the peculiarities of their constituent minerals. The rocks represented here belong to the various horizons already mentioned, and include gneiss, ferruginous gneiss, chlorite slate, quartzites, and hydro-mica slates, limestones, dolomites, ferruginous conglomerates, quartz conglomerates, " Potomac marble" (nether member of the Mesozoic series), dolerites, and a syenite. The order in which these are named is, roughly, the order .of geographical position in a section line from southeast to northwest, commencing at the intersection of the Northern Central Railroad with the Maryland line, and ending a few miles from the town of York, and a short distance within the marginal outcrop of Mesozoic red sandstone. In such a geographical section all the rocks above mentioned would be encountered in the given order except syenite, about which a few words are to be said in a moment. (But this is far from representing the rocks in their geological sequence.) There is nothing of unusual interest to present to your notice in these slates and quarteites. The limestones were carefully searched tinder 450 diameters microscopic power, but they show no signs of organic remaius. One section of a fine-grained Triassic sandstone contains a very beau- . tifully banded plate of quartz. But the objects of greatest interest at present are the specimens of trap. The more fine-grained and compact traps were collected from

By C. P. Watson

It is perhaps significant that a few years ago the sessions held here were chiefly occupied with production. In the last two years these sessions have been concerned with production curtailment, unitization and conservation, notwithstanding that production in the United States in 1929 reached a total in excess of 1,000,000,000 barrels. A study of the leading producing units in the United States shows that Oklahoma, Texas and California in 1929 yielded 84 per cent. of the total production from 33.5 per cent. of the total number of producing wells. Production in the United States in 1929 showed an increase of 107,000,000 bbl. over the 1928 figures. This increase in itself perhaps is not enough to have caused the serious situation that is now confronting the industry. However, taking into account the gradual encroachment on the consumption of fuel oil through the greater utilization of natural gas, probably we have reached the point in the United States where prices will determine to a large extent,' in 1930, the amount that will be produced. In the states of Texas, Oklahoma and California, the most significant developmcnt of 1929 has been the desire of operators to reach some agreement to bring production more or less in control with the estimated demand. In November, production in California, particularly in the Santa Fe Springs field, was drastically cut to meet a certain requirement. Similarly, in Texas, the Yates field has been developed and has been producing under an agreement on the part of the operators; and more recently in Oklahoma City, serious efforts have been made to keep produetion in line with consumption. For the year 1930 we can see nothing in sight except drastic curtailment. This is a matter that I am sure is occupying the attention of all the leaders of the industry.

Jan 1, 1930

By J. Chipman, J. C. Fulton

Reduction of Si from slag to carbon-saturated iron is a very slow reaction. The rate is nearly independent of stirring but is accelerated markedly by increased temperature. In a slag containing 45 pct SiO2, 38 pct CaO, 17 pct Al2O3, the energy of activation is approximately 130 kcal. AT temperatures of 1450" to 1600°C occurring in the hearth of the iron blast furnace, chemical reactions are normally expected to proceed with great rapidity. Many of the reactions of iron making are indeed quite rapid and attain a condition corresponding roughly to a state of equilibrium before metal and slag are tapped from the furnace. The one conspicuous exception is the reaction by which carbon in the coke or metal reacts with silica in the slag to deliver silicon to the metal. From the practical viewpoint the slowness of this reaction is indeed fortunate, for if it were fast enough to reach equilibrium during the time of contact, it would be difficult to produce pig iron of the desired low silicon content. The one other reaction which under certain circumstances can also be very slow is the transfer of sulfur from blast-furnace metal to slag. In their laboratory exeriments on this reaction, Hatch and Chipman found that at least 5 hr were required for the attainment of equilibrium in a small crucible and that the reaction was not accelerated by increasing the rate of stirring. Subsequently it was shown2 that the presence of a reducible oxide MnO greatly inhibited sulfur removal, and finally that SiO2 itself3 under some conditions has sufficient oxidizing Dower to interfere with sulfur transfer. The kinetics of sulfur removal are now rather well understood,4 and it has been shown3,5 that when the silicon content of the metal is high enough to prevent reduction of SiO,, the desulfurizing process is rapid. Thus the observations of slow removal of sulfur are associated with the coincident slow reduction of SiO2, a process which transfers both silicon and oxygen to the metal phase. It is, of course, the oxygen which interferes with sulfur removal. An explanation of the slowness of the silica reduction reaction has not been obtained. The sulfur transfer process has been shown by the authors5 to be at least partially transport-controlled in the absence of interference by silica. Under the experimental conditions. 99 pct of the total transfer at 1600" was accomplished within an hour. Under similar conditions the reduction of silica may not proceed half-way to equilibrium6 in 8 hr. It is scarcely imaginable that silica reduction could be transport-controlled when the slag contains 44 pct SiO2 and the metal about 1.4 pct C. The experiments reported here show definitely that it is controlled by a slow step or steps in the chemical reaction. One might expect to find such a slow step in the breaking of SiO bonds or in the slow removal of oxygen by carbon at the slag-metal or metal-crucible interface or by bubble formation. EXPERIMENTAL PROCEDURE The experimental procedure used in this investigation was similar to that used in the study of the kinetics of desulfurization.5 A sketch of the graphite crucible and stirrer used in the current work is shown in Fig. 1. The quantity of metal and slag used was adjusted so that the slag-metal interface was located between the top and bottom blades on the stirrer; the top of the slag layer was above the top blade. The stirrer shaft was hollow down to the metal level and served as thermocouple well or optical pyrometer target. Stirring speeds of 0 to 500 rpm were used. A carbon monoxide atmosphere was maintained in the furnace by flushing the gas over the slag surface, except in run No. 220 when it was bubbled

Jan 1, 1960

By Robert B. Hall, Charles W. Bauer

Alunite, KA13(SO4)2(OH)6, was used from the 15th century until early in the present century as a source of potash alum and aluminum sulfate. Since early in this century its use for this purpose has declined to virtually nil with acid treatment of bauxite or clay replacing alunite as a source of alum. During the First World War alunite served as an emergency source of potassium sulfate fertilizer in the United States and Australia. More recently, alunite has been investigated as a nonbauxite ore of aluminum, with potassium sulfate and sulfuric acid as recoverable byproducts. The Soviet Union established a commercial-scale plant in the mid-1960s producing cell-grade alumina from alunitic ore and recovering byproduct potassium sulfate and sulfuric acid. Interest in nonbauxite ores, including alunite, is expected to continue in countries that presently are dependent on imports of bauxite or alumina to support their aluminum industries. The US has the largest aluminum producing and fabricating industry in the world but imports more than 90% of its aluminum-bearing raw materials. This chapter reviews the status of alunite as a potential source of aluminum with byproduct fertilizer, and the resources available to support this industry, whenever this becomes economically feasible. Historical Background Alunite has received little attention until recently, yet for centuries it held a higher place than many of the industrial minerals considered essential today. The deposits of alunite at Tolfa, northwest of Rome, were mined almost continuously from 1462 until about the middle of the present century (DeLaunay, 1907; Lombardi, 1977). The potash alum made from the alunite, called Roman alum, was a valued commodity in international trade, being used in the making of paper, in tanning leather, and as a mordant in textile dyeing. The industry at Tolfa is said to have been controlled by the Vatican and was a source of revenue for the Papal State until fairly recent times (Lombardi et al., 1977). Since early in the present century, the preferred method for making alum has been by acid treatment of bauxite, clay, or other aluminous material, so that alunite has fallen into near-total disuse as a source of alum chemicals. Appreciable quantities of mixed alunite-kaolin rock still are quarried in the Tolfa district for use by the Italian cement industry (Lombardi and Mattias, 1979), but the role of this material in the making of Italian cement is not clear. A large deposit of alunite-bearing rock in Chekiang province, mainland China, is said to have yielded a "great quantity" of alum over a period of several centuries (Yih, 1931). During the 19th century, alunite deposits in France, Spain, Australia, and other countries were exploited as raw material for making potash alum and aluminum sulfate. Interest in alunite was revived during the First World War, not for alum, but as an emergency source of potassium sulfate fertilizer. Large veins of nearly pure alunite had just been discovered on Alunite Ridge, 11 km southwest of Marysvale in Piute County, Utah (Butler and Gale, 1912), and these were quickly brought into production for making potash fertilizer to replace supplies cut off from the famous deposits at Stassfurt, Germany. An estimated 225 kt of Marysvale alunite was mined and processed at that time (Callaghan, 1973). Similarly, Australian alunite deposits were mined as a source of potash fertilizer during both world wars (Hall, 1978).

Jan 1, 1983

By I. R. Kramer, H. Shen, S. E. Podlaseck

The tensile and creep properties of aluminum in vacuum have been investigated. It was found that the general effect of a vacuum environment was to reduce the rate of work hardening. Results obtained from creep tests showed that lowering the test pressure from 2 x 10-4 to 10-7 torr produced a decrease in the activation energy as much as 500 cal per mole. An attempt is made to explain these effects in terms of how the surface-stress field of a specimen may be affected by a vacuum environment during plastic deformation. In a previous paper,' the results were reported of some of our early work on the effect of vacuum environment on the stress-strain curve of aluminum single crystals. This effort has been extended to the studies of the tensile and creep properties in vacuum as a function of various metallurgical parameters. Some of the recent surface-effect studies2'3 have revealed that a region of high dislocation density, the so-called "debris" layer, is formed near the surface of the specimen as a result of plastic deformation. This layer acts as a surface barrier to oppose dislocation movement. The strength of this barrier depends on the surface condition such as oxidation or surface removal. Experimental results obtained from surface-removal work2, 3 indicate that such a surface barrier, which may be characterized by a stress field, affects the applied stress and the rate of work hardening. In the case of aluminum, this stress field was found to be directly proportional to the strain and the strain rate; however, the slope of this curve is independent of orientation of the crystal and may be altered by using different surface treatment. Since the escape of dislocations may be retarded by the presence of an oxide on the surface of a specimen, it is expected that a change in the rate of oxidation in vacuum will affect the process of dislocation accumulation in the debris layer. Consequently, it also affects the plastic behavior of a metal. This paper reports the changes in some of the creep and tensile properties of aluminum in vacuum and discussions of the observed effects in terms of the concept of the "debris" layer. EXPERIMENTAL PROCEDURE Tensile Tests. A sketch of the tensile apparatus is given in Fig. 1. This apparatus was contained in a bell jar (14 in. diam by 24 in. high) connected to a 10-in. vacuum system. The load was applied to the specimen by means of a gear train which was driven by a magnetic clutch located outside the vacuum chamber. The specimen, held by a pair of square shoulder grips, was attached to the load cell at the top and the drive gear at the bottom. A displacement transducer was placed between the two grips as shown in the figure to measure the elongation. Signals of elongation and load were amplified and recorded on an X-Y recorder. The system was capable of detecting loads as small as 0.025 lb and displacements of 0.0002 in. Shoulder-grip specimens of aluminum single crystals, having a nominal square cross section of 1/8 by 1/8 in. and a 3-1/2-in, gage length, were grown by the Bridgeman techniques. The original purity was 99.997 pet. The orientations of the crystals investigated are shown in Fig. 4(a). The crystals were annealed at 600°C for 2-1/2 hr, electropolished, and placed in the vacuum test chamber without any delay. All the crystals were deformed at a strain rate of 4 x 10-5 sec-1 at 24o ± 3°C. A study was made to find whether a chemically passive surface film would give the same effect as a vacuum environment. Specimens of aluminum 1100 (0.187 in. diam with a grain size of 0.1 mm)

Jan 1, 1965

By M. H. Caron

THE most outstanding property of ammonia liquors, used in the ammonia leaching process is their very limited ability to dissolve all compounds present in reduced ore except nickel and cobalt. Although they do have such a high degree of purity, even the smallest amounts of impurities contaminate the precipitate of basic nickel carbonate that may be obtained from pregnant liquors by straight distillation. Figures have been given in a separate paper regarding the extent of such contamination. The product of straight distillation is likely to contain small amounts of Fe, Mn, MgO and SiO2 as well as some sulphate and sulphide. The sulphur can be readily eliminated by calcination of the product at the proper temperature and MgO and SiO2 by reduction and melting of the metal with a suitable flux. After such treatment the metal is relatively pure, and the iron and manganese content will be very small. The cobalt content, however, may vary considerably, depending upon the ore treated. The metal obtained from pure true garni-erite ores usually has only a small cobalt content of less than 1 pct. Metal obtained from medium grade iron-rich nickel ores may show cobalt values from 2 to 3 pct, and the alloy obtained from laterite is likely to contain as much as 10 pct cobalt. By proper treatment a good deal of cobalt may be recovered from lateritic nickeliferous iron ores, and cobalt will become the major constituent of the pregnant liquor if asbolan ores or similar products are treated. The pregnant liquor of "run of mine" nickel ores may have a pinkish shade, indicating the presence of cobalt. It is evident that from such liquors the metals should be recovered separately. Even if cobalt is present in only very small amounts, it would probably be economically justifiable to recover both metals as pure as possible if a suitable process could be devised. The author has made investigations along this line and has patented some processes adapted to the treatment of this type of solutions. Selective Dissolution of Nickel from Basic Nickel Carbonate Containing Some Cobalt: Basic nickel carbonate obtained from true garnierite ores by straight distillation of the pregnant liquors, always contains some cobalt as well as the normal impurities. In. order to improve the quality of the nickel product and to recover most of the cobalt, the following process has been devised. By using liquors with a low CO2 to NH3 ratio, nickel can be redis-solved preferentially to cobalt. It is not a sharp and clean separation but a selective one, for the bulk of the nickel may be redissolved with a small amount of cobalt, and a small residue may hold the bulk of the cobalt. The greatly increased cobalt content of the residue is indicated by a pronounced olive green color, in contrast with the light green color of pure basic nickel carbonate. The following example is given from Dutch patent No. 52788, Klasse 40a. 43 granted June 17, 1942: The original precipitate contained about 0.55 pct cobalt calculated on total nickel + cobalt. Eight hundred and fifty grams of the basic nickel carbonate were redissolved in leach liquor containing 7.12 pct NH3 and 2.12 pct CO2. The weight of the dry residue was about 3.5 pct of the original weight. By analysis it was found that the residue contained: Fe 1.93 pct, Co 6.01 pct, Ni 34.87 pct and also a certain amount of silica. The clear filtered blue liquor was distilled and the precipitate of basic nickel carbonate from this analyzed: Fe 0.008 pct, Co 0.0146 pct, Ni 42.37 pct. It is obvious that this product is considerably more pure, since calculation shows that about 94 pct of the original cobalt remained in the residue. Cobalt and nickel can be recovered by further

Jan 1, 1951

By J. Lemish

Considerable research has been conducted in Iowa in recent years on carbonate aggregate reactions in concrete. Groups outside the state have become active in the past few years after recognizing that certain carbonate aggregates are reactive in concrete. The paper reviews the nature and extent of the problem and a summary is given of research by the author and his associates. In recent years considerable research has been conducted in Iowa on carbonate aggregate reactions in concrete. The research is part of a general study on the behavior of carbonate rocks as concrete aggregates sponsored by the Iowa State Highway Commission. Research on carbonate aggregates has not been extensive in the past. Laughlin1 published one of the first papers on carbonate aggregates in 1928 and was followed by others, notably H. S. sweet,' B. Mather et al.,3 and K. Mather4 who emphasized the petrographic and physical aspects of carbonate aggregates. The recognition that certain carbonate aggregates are reactive in concrete has led to increased participation in research in the past few years by groups outside of Iowa. Significant contributions have been made by Swenson and Gillot,5 Hadley,6 and Chaiken and Halstead7 in work which emphasizes the expansion of carbonate rocks in alkaline environments and the reaction of carbonate minerals or dedolomitization with alkalies. It is the purpose of this paper to review briefly the nature and extent of the problem and present a summary of the research by the author and his associates. EXTENT AND NATURE OF THE PROBLEM The problem is the deleterious behavior of certain carbonate aggregates in concrete. It was first recognized in Iowa over 20 years ago when poor service records of certain highways were correlated with aggregates produced from the Glory and LeGrand quarries. Deleterious behavior of carbonate aggregates have been reported in Canada and, more recently, in New York and Virginia. As more knowledge is gained concerning the problem, distress in concrete related to carbonate aggregates may be recognized over a widespread area. The problem may potentially exist in the Midwest, the Northeast, and other parts of the country underlain by thick sections of carbonate rocks readily available for utilization as aggregates. The nature of distress in Iowa highways is a general weakening and deterioration of concrete characterized by progressive cracking and spalling away from joints and edges (Fig. 1). The distress generally occurs after 15 years of service and becomes progressively worse. Specimens of such concrete lack the toughness of sound concrete and break easily under the hammer in the manner of a soft brick. The matrix is generally highly carbonated and dark borders, or reaction shells or rims outline the argillaceous carbonate aggregate fragments (Fig. 2). Cracks observed in cores cut across the aggregates and concrete matrix. Although localized volume change (expansion) is associated with spalling, there is no definite field evidence in Iowa that excessive growth of concrete slabs has occurred. The experience with carbonate aggregates in Iowa indicates that the concrete deterioration is not the same as that induced by the alkali-aggregate reaction associated with siliceous aggregates. The principal difference is that in Iowa the distressed concrete is weakened throughout the slab. In concrete affected by the alkali aggregate reaction, the

Jan 1, 1961

By J. P. Givry

The bath and the liquid metal in the aluw~inuw~ electrolytic cells are moving under the action of the Laplace forces. Consequently there are differences in level at the interface of the liquid. This phenomena is studied by means of a computer; the characteristics of the mathematical model used are presented with the results corresponding to two typical cases. This study gives a new and origi~zal interpretation of magnetic ej-jects; their action depends very closely on the hydraulic phenomenon which explain the sensibility of the cells to the slope and thickness of solid bath frozen around the pot. MAGNETIC effects produced in the electrolytic cells used for the production of aluminum are known to exist, a factor whose importance is well-known by producers through its influence on cell operation and output. In particular, these effects bring about movements in both the bath and metal as well as interface variations in level that are detrimental to sound electrolysis . A direct study of these effects by means of an experimental device would raise a number of problems particularly difficult not to say impossible to solve in the present state of techniques. It is for this reason that we had recourse to an electronic computer for working out the speed and pressure distribution within the liquid in the cells. We have assumed that all other possible causes for movement, such as thermal convection and evolution of gas at the anode, are acting without any connection with magnetic effects, and that consequently we may study each of these causes separately. A basic cause for magnetic effects lies in the presence of Laplace forces within the bath and metal. Electric current and magnetic field distribution have been calculated with the help of an electronic computer, and two communications about it have already been made to AIME.* 1) PRESENTATION OF THE MATHEMATICAL PATTERN In order to solve this problem, it was essential to assume a number of simplifying hypotheses with regard to both the geometry of the actual cells and the phenomena themselves. A first simplification consisted in assuming that the movements of the conducting liquid modify neither the electric currents nor the magnetic fields. In consideration of the magnitude of the values involved this assumption seemed accep-tible. 1.1) Finding the Equation of the Problem. The problem raised consisted in determining the flow of two viscous immiscible liquids with different densities subjected in a complex environment to gravity and Laplace forces. As a matter of fact, the sum of the external forces acting on the liquids is: F = JAB +pg where F = volume energy, B = magnetic field, J = current density, p = specific gravity, g = gravity. In the case of a laminar flow and assuming that the liquids are Newtonian and incompressible liquids, the equations governing movements are the following: 1) Navier Stokes' equation written in vectorial form: In fact one tries to find a steady-state solution, so aVx/at = 0; besides, one assumes that the movements are slow enough for quadratic terms such as Vy(a Vx/ay) (of round about the square of speed) to be neglected in front of the viscosity term: pAV, so

Jan 1, 1968

By Pramod C. Thakur

Introduction Methane is contained under pressure within the fractures and adsorbed on the surface of the coal seams and adjacent strata. It is released into the mine atmosphere during mining of the seam creating explosive gas-air mixtures. Large volumes of air, sometimes as high as 20 tons of air for each ton of coal mined, are circulated constantly to dilute and carry away methane from coal mines. Removal of methane from solid coal, wherever high methane emissions occur, has been discussed by Spindler and Poundstone (1960) and Thakur and Davis (1977). Methane control in longwall gobs is much more complicated. As longwall mining progresses, the overburden continually subsides, and the immediate roof caves behind the roof supports. Even the underlying strata heave and open up communication channels feeding gas to the longwall gobs. The pressure of gas in the underlying and overlying strata is usually higher than the ambient air pressure in the mine. Thus the mine workings become natural pressure sinks, into which gas flows from the entire disturbed zone. Winter (1975) defines this zone as the "gas emission space". Depending on the number of gas-bearing zones in the gas emission space and their gas contents, the total methane emission from longwall gobs could vary from a few to more than one hundred cubic meters of gas per ton of mined coal. Hence the ventilation of longwall faces demands a large quantity of air. This ventilation need is further enhanced by high air losses specially on caving faces (with no stowing of the gobs). The old system of longwall ventilation, the 'U' pattern, where all the air was brought down one gate road and exited through the other gate road, loses large quantities of air through gobs giving a high methane concentration at the return end of the face. The 'Y' ventilation pattern where intake air is brought down both head and tail gate roads relieves the situation to some extent but, on most longwalls, some kind of methane control is still needed. With the onset of longwall mining in Europe several decades ago, the initial work on methane control on longwall has naturally been done there. The basic principle of methane control has always been, and still remains, some means of "bypassing methane from the gas emission space without letting it mix with the mine air". In most cases the bypassing mechanism is either a strategically located borehole or a roadway. A successful methane control program depends on the following basic premises: a. Determination of the geometry of the gas emission space and location of gas bearing horizons therein. b. Estimation of the rate of methane influx into the longwall gob. c. A scheme to bypass the gas in the most economic and efficient manner and thus prevent it from entering the mine atmosphere. In successful methane drainage programs a high proportion, usually between 50 and 70 percent, of the total gas emissions in a working district is removed before it can enter the mine airways. Advantages of methane drainage can be summarized as: 1. Generally reduced methane levels in the mine leading to increased safety and productivity. 2. Reduced air requirements and corresponding savings in ventilation horsepower. 3. Faster rate of advance for development headings and economy in the size of headings. 4. Possible use of mine gas as an additional source of fuel. The purpose of this paper is to briefly review the geometry of gas emission space and methane influx therein and discuss more successful European and U.S. longwall gob gas control techniques.

Jan 1, 1981

By B. H. Kear, H. G. F. Wilsdorf

After a few percent strain, dislocations in disordered Cu3Au are arranged in groups in ulell-defined slip planes, which contrasts with the more or less random distribution of dislocations in the corresponding ordered alloy. Unusually long and straigkt dislocation segments observed in the ordered alloy are interpreted in terms of cross slip of screw dislocations from their slip planes into cube planes. It is proposed that cross slip, and also dislocation reactions of the Lomer type, play an important role in work hardening of the ordered alloy. ACCORDING to to dislocations in the disordered lattice are only partial dislocations in the corresponding super lattice, so that in the super-lattice dislocations must occur as pairs, with each pair connected by a ribbon of antiphase boundary. Recently, striking confirmation of the theory was obtained by Marcinkowski, Brown, and Fisher3j4 in a study of dislocation configurations in thin foils of the Cu3Au alloy by transmission electron microscopy. In the present investigation, the observations made by these workers have largely been confirmed. Moreover, it has been found that dislocations in the plastically deformed ordered alloys are often unusually long and straight. This paper is mainly concerned with these new observations. A tentative explanation is offered in terms of cross slip of dislocations in the ordered alloys. PREPARATION OF SPECIMENS An alloy close to the stoichiometric composition Cu3Au was prepared by melting together high-purity copper and gold (99.995 pct) under vacuum in a graphite mold. The resulting ingot was rolled down and cut into strips 1 1/2 by 1/8 by 0.005 in. in thickness. All strips were annealed at 900°C for 3 hr and cooled to 500'~. A few of the strips were quenched from ~OO'C, while the remainder were slowly cooled in the temperature range 400" to 150°C at intervals of a few degrees every 24 hr to produce a high degree of order. After this annealing treatment the average grain size of the material was about 0.1 mm. Material in different states of order was obtained by reannealing fully ordered material at temperatures below the critical temperature: followed by quenching. The equilibrium degree of order attained at a particular reannealing temperature was obtained from the paper by Keating and warren.' A simple hand-operated tensile jig was used to give the strips the required amounts of plastic strain. Following straining, a number of specimens were cut from each strip by means of an electrolytic cutting device.= Finally, each specimen was thinned electrolytically using the polishing procedure described by Bakish and Robertson,7 and these thin sections were examined in the Philips EM-100B electron microscope operating at 100 kv. EXPERIMENTAL OBSERVATIONS Antiphase boundaries. The average domain size in the ordered alloys was found by direct observation to be about 0.25 p. Also, it was observed that the grown-in configuration of antiphase boundaries was changed little by plastic deformation, at least up to 6 pct strain. Fig. 1 shows an electron micrograph of a thin foil of partially ordered alloy (S - 0.8) after 3 pct strain. The micrograph shows a few dislocation pairs and a somewhat crystallo-graphic network of antiphase boundaries. The normal to this foil was found by diffraction analysis to be approximately 11121, with principal directions in

Jan 1, 1962

By E. A. Elevatorski

Wollastonite, named after William H. Wollaston, an English chemist, is a calcium metasilicate, CaSiO3. It has a short history as an industrial mineral. The earliest production of wollastonite is reported to be from a deposit near Code Siding, located north of Randsburg, Calif. At this locality small tonnages of wollastonite were quarried during 1933-34 and 1938-41, and processed into mineral wool. This operation was largely experimental and virtually no United States production was again reported until the 1950s when a large deposit near Willsboro, N.Y., was developed by the Cabot Corp. A processing plant was placed on-stream in 1953, with nearly continuous production to date, and it is currently operated by Interpace Corp. Since 1958, wollastonite deposits in the Little and Big Maria Mountains of Riverside County, and in the Panamint Range of Inyo County, both in California, have operated intermittently for production of both ornamental and commercial wollastonite. During 1973, the United States was the major producing country, furnishing about 75% of the world's output. Recent production also has come from Finland, Mexico, and Kenya. Small amounts have been shipped intermittently from India, USSR, New Zealand, Republic of the Sudan, Republic of South Africa, and South-West Africa. The principal use of wollastonite is in the manufacture of ceramics, especially wall and floor tiles. Other uses are for paints, fillers, adhesives, reinforcing agents, plastics, fluxes, and glazes. Mineralogy Pure wollastonite, CaSiO3, has the composi¬tion of 48.3 % CaO and 51.7 % SiO,. However, it is seldom found in the pure state due to the ease with which it takes into solution the metasilicates of manganese, magnesium, iron, and strontium. Predominantly, wollastonite occurs as a contact metamorphic deposit forming between limestones and igneous rocks. Commonly associated minerals are garnet, diopside, epidote, calcite, and quartz. It has a specific gravity of 2.8 to 3.0, and hardness of 4.5 to 5 on Mobs' scale. When pure, it has a brilliant white color, but with impurities it may be grayish or brownish. Luster is vitreous to pearly. Melting point of wollastonite is about 1540° C. Wollastonite occurs in coarse-bladed masses, rarely showing good crystal form. It is usually acicular or fibrous, even in the smallest of particles. The most unique property of crushed and ground wollastonite is its cleavage. Fragments of crushed wollastonite tend to be needle-shaped, imparting a high strength, and this property is the basis for many of its uses. The fiber lengths are commonly in the ratio of 7 or 8 to 1, length to diameter. Some crystals of wollastonite fluoresce under short-wave or longwave ultraviolet light, or both; colors ranging from yellow-orange to pink-orange. Specimens may also show phosphorescence. The brightness of wollastonite is a property of considerable importance to the paint industry. Material, 99% pure, with a size of -325 mesh, has a General Electric reflectance rating of 92 to 96%. Chemically, wollastonite is inert and this property makes it useful as a filler and reinforcing agent. There are two polymorphs of calcium silicates: wollastonite, a low temperature form, and pseudowollastonite, a high temperature form. Inversion of wollastonite to pseudowollastonite occurs at about 1120° C, resulting in an increase in the coefficient of expansion and a color change. Pure white wollastonite, on inversion, may change to a cream tint, or various shades of red or brown. The color change is thought to be due to the presence of iron and strontium.

Jan 1, 1975

By C. S. Brooks

Several of the commonly used methods for deter-mination of effective grain densities of minerals have been evaluated for accuracy and precision, and their applicability to various types of petroleum reservoir minerals tested. Consideration was given to the effect of consolidation, swelling clay, and wettability on these grain-density determinations. Procedures with helium displacement, a modified low-pressure Boyle's law porosimeter, and liquid displacement (water, n-decane, and n-octanol) were tested. The helium-displacement procedure was used primarily as an independent reference for which the effects of fluid-solid interaction, e.g., adsorption and wettability, were negligible. The procedures with the Boyle's law porosimeter and with liquid displacement are the methods in common use. Minerals investigated included calcite, West Texas limestone core samples, California sandstone core samples, and Wyoming bentonite. The number of samples tested, while not large, was adequate to permit application of statistical methods. Grain-density measurements on calcite (Iceland spar) provided a basis of comparison for the accuracy and precision of the procedures under investigation for a material with a high degree of chemical and physical homogeneity and for which fluid-solid interactions were at a minimum. Liquid-displacement procedures (water or n-decane) provided the greatest reliability and precision for measurement of the grain densities of the limestone tested. Gas-displacement procedures (helium or Boyle's law porosimeter) provided the greatest reliability and experimental convenience, if not the greatest precision, for the measurement of the grain densities of the swell- ing clay, Wyoming bentonite, and the shah sandstones which -contained appreciable amounts of swelling, in-terstitial clays. These experiments were designed to evaluate the applicability of the grain-density procedures in common we to some of the less tractable minerals—tight limestones, shaly sandstones, and swelling clays. The results should provide a useful basis for a selection of the method most suitable for application to the various petroleum reservoir minerals encountered and especially for use in the estimation of formation porosity. INTRODUCTION These experiments were undertaken to evaluate the accuracy and precision of several commonly used methods for determination of effective grain densities of minerals, and to test their applicability to various types of petroleum reservoir minerals. Consideration was also given to the effect of consolidation, clay, and wettability on these grain-density determinations. Procedures used included measurements with helium displacement, with a modified low-pressure Boyle's law porosimeter, and with liquid displacement (water, n-decane, and n-octanol). The minerals investigated included calcite, West Texas limestone core samples, California sandstone core samples, and Wyoming bentonite. The accurate determination of the porosity of petroleum reservoir formations, in particular those of low porosity, has received much attention. Both bulk-volume and grain-volume measurements necessary in the evaluation of porosity have been examined by many investigators with the objectives of improving both the accuracy and the precision of these determinations. In this investigation statistical criteria for selection of the most reliable and suitable procedure for use with a given type of mineral are demonstrated. The grain-volume measurement procedures appear to be the most susceptible to improvement.

Jan 1, 1958

By C. H. Li, J. A. Sarteli, W. Bonfield

The stress to cause a permanent micros train of 2 x 10-6 in. per in. (defined as the microscopic yield stress) in beryllium is found to be very sensitive to surface condition. The initiation of plastic flow in as-machined specimens, which contain a high density of twins and large residual compressive stresses to a depth of about 0.010 in. from the surface, occurs by the nucleation of slip from high stress fields around twin tips in the surface layers. Removal of the damaged surface layers by chemical polishing results in an appreciable increase in the microscopic yield stress, which is attributed to the remoual of stress raising twins rather than to the release of residual stresses. IT is well known that the macroscopic mechanical properties of beryllium are very sensitive to the nature of its surface finish. Matthews and coworkers1 have shown that the tensile strength of rolled beryllium sheet can be considerably enhanced by chemical polishing, presumably due to the removal of the high concentration of notches, twins, and large residual compressive stresses normally found in the surface layers of ground specimens. There was no similar effect of surface condition on the macroscopic yield stress (the stress to produce 0.2 pct strain), a point to which we shall return. To date there have been no extensive studies on the effect of surface condition on the microstrain region of beryllium. Recent measurements2 of the stress to cause a permanent microstrain of the order of 10-6 in. per in. on machined hot pressed QMV beryllium, gave values ranging from about 600 to 3500 psi. Reasons for the considerable scatter in the results were not discussed. In this paper, we wish to show that the microstrain region of polycrystalline beryllium is, in fact, very sensitive to surface condition. The stress to cause a permanent strain of 2 x 10-6 in. per in. which for convenience we will refer to as the microscopic yield stress, can be increased by almost a factor of 2 by minimizing the amount of surface damage. The variation of microscopic yield stress is attributed to the presence of twins in the surface layers, rather than to residual compressive stresses. EXPERIMENTAL PROCEDURE The starting material for this investigation was commercial purity hot pressed QMV beryllium, with an average grain size of about 20 . The effects of surface treatment were assessed by comparing the microstructure with residual stress measurements and microstrain properties. Specimens were prepared for metallographic examination by wet grinding with 240, 400, and 600 papers, followed by polishing with a suspension of fine alumina in warm 20 pct oxalic acid. After this treatment, the surface could be examined, either in the unetched condition with polarized light, or after etching in 2 pct hydrofluoric or boiling 20 pct oxalic acid with normal light. Thin films of beryllium suitable for electron transmission study were prepared from bulk specimens by chemical polishing with hydrofluoric and phosphoric acids, and were examined in an RCA-EMU-3 electron microscope. Residual stress measurements were made by a procedure similar to that of Treuting and Read.3 Specimens 4.0 in. by 0.625 in. by 0.080 in. were prepared by three different machining procedures, namely: turning, grinding, and sawing, in order to introduce different levels of residual stresses. An electrical resistance strain gage was attached to one side of the specimen, and that surface was then protected by an acid-resistant enamel, while the opposite surface was removed by etching approximately one thousandth of an inch at a time. The change in specimen curvature in the longitudinal direction was noted and the residual stress was calculated by the following formula:

Jan 1, 1963

By D. F. Kaufman, E. D. Levine, L. R. Aronin

The deformation of' impure beryllium crystals by basal glide at room temperature invariably tevminates by basal cleavage after a few percent strain. It is generally accepted that .fracture of this type is caused by the splitting of low) -angle boundaries, or bend planes, by obstacles that restrict the motion of the bed planes in the deforming crystal. The details of such a process have been developed by Stroh, who showed that the high tensile stress norrnal to the basal plane in the region where the bend plane is split results in the propagation of a basal cleavage crack, provided there is no available dejorvrlatzon mode having a shear component normal to the basal plane It has been postulated that puvification of beryllium might lead to increased basal ductility by the vemoval of barviers to bend plane motion and possibly by the activation of nonbasal defor~rlation systems. Large increases in the amount of basal glide that can he sustained prior to fracture have been observed in crystals purified by zone refining. In each case, eventudal fracture was by sharp basal cleavage, suggesting that the split bend plane model still applies to tile fracture of beryllium of rensonably high purity. In the present work, calculations are made to show to what extent basal duetilits can be increased by purification while the split bend plane .fracture process remains applicable. Experimentally observed ductilities are generally somewhat lower than those predicted by calculation because of premature failure due to defects introd~cced during specimen preparation and testing. SEVERAL investigators1-4 have studied the deformation characteristics of beryllium single crystals of commercial purity, and have related the strong anisotropy of plastic deformation in single crystals to the problem of brittleness in polycrystalline beryllium. For most orientations, the principal deformation mode is basal slip, which, at temperatures between 300" and 900°K, begins at a critical resolved shear stress of approximately 1500 g per sq mm and terminates after 3 to 6 pet glide strain by cleavage on the basal plane in the neighborhood of (1120) bend planes that are formed during the deformation. This type of fracture, which is also observed in zinc at low temperatures, has been interpreted by stroh5 to be caused by the splitting of bend planes by obstacles to their motion. In the Stroh model, a (11.20) dislocation wall, or bend plane, moving along the slip direction under the action of the applied stress, encounters obstacles which cause part of the bend plane to be held up, the other part continuing to move. Stress concentrations are built up in the region where the bend plane is split, with a high tensile component normal to the basal plane, resulting in a microcrack at the end of the split wall. Because no deformation mode having a shear component at an angle to the basal plane is available to relieve the stress at the crack tip, the crack can propagate under a sufficiently high applied stress. The Stroh criterion for crack propagation is given by

Jan 1, 1964

By C. W. Spencer, Che-Yu Li, R. J. Knight

The usual reaction product for the monotectic reaction in the Bi-Se system consists of rod -shaped particles of selenium-rich liquid embedded in a single crystal matrix of At certain crystallo-graphic orientations of the matrix with respect to the reaction interface, more complex shapes are as -sumed by the liquid particles. This reaction has been examined at different growth rates and relative crystallographic orientations of the matrix with respect to the reaction interface. The uhriation in auerage particle size of the liquid phase with reaction rate has been determined at one crystallograpIzic orientation of the matrix. On a plot of logarithm of average particle diameter vs logarithm of reaction rate, data points for crystals grown at rates of 10- to 1.0 cm per hr fall near a curve of slobe -0.4. MONOTECTIC reactions in binary alloy systems are reactions of the eutectic class in which, as the system is cooled through the three-phase reaction isotherm, one liquid phase (L) decomposes to a solid phase and another liquid phase (LII).' A partial phase diagram, as taken from Hansen, showing the monotectic reaction in the Bi-Se system is given in Fig. 1. This diagram specifies the monotectic point at 618°C and 72 at. pct Se, and the monotectic reaction products as the intermetallic Bi Se3 and a liquid (LII) which contains approximately 98 at. pct Se. At a lower temperature, 217°C, this liquid may undergo a eutectic reaction in which the reaction products are BizSe3 and crystalline selenium. However, under conditions of rapid cooling, or quenching, from above 217°C, this selenium-rich liquid may be partially retained to room temperature in an amorphous or glassy state. The intermetallic BizSe3 is rhombohedral, of the space group jm;' however, for convenience it is usually represented by a hexagonal struture. A pronounced plane of cleavage, which lies perpendicular to the main axis of the rhombohedral unit cell or parallel to the basal plane of the hexagonal cell, exists in the structure. The usual monotectic reaction product consists of rod-like particles of LII embedded in a single-crystal matrix of BizSe3, although at certain crystallographic orientations of the matrix BizSe3 other more complex shapes are assumed by LII. A similar rod-like, or cylindrical, morphology for the carbide phase has been reported by westbrook7 in the a Cr-Crz3Ce eutectic structure. In this paper the morphological characteristics of the LII particles, as retained to room temperature, have been examined under conditions of varying growth rate and crystallographic orientation of the matrix BizSe3 with respect to the growth direction. EXPERIMENTAL PROCEDURE Alloy specimens corresponding to the monotectic composition, 72 at. pct, or 50 w pct Se, were prepared from 99.999 pct pure bismuth and selenium obtained from the American Smelting and Refining Co. The two elements, corresponding to a total specimen weight of approximately 30 g, were encapsulated in 13 mm OD Vycor tubing under a vacuum of 5 x X mm of Hg. The capsules were suspended on a fine platinum wire in a Bridgman-type furnace which exhibited a temperature gradient of

Jan 1, 1963

By T. S. Spice, H. L. Lovell, R. W. Utley

With the increased demand for lightweight aggregate, such materials have been manufactured from slags, clays, slates and, to a minor extent, the refuse of coal preparation processes. The latter source is attractive due to current interest in eliminating air pollution and improving the unsightly appearance of refuse piles as well as potential economic advantages, if a satisfactory product can be manufactured. A study has been made relating the composition of coal refuse, expressed as washability data, and the properties of a resulting aggregate. Three different refuse samples (bituminous and anthracite) were separated at gravities ranging from 1.4 to 2.96. Their chemical composition was determined. Aggregates were prepared in the laboratory from these fractions before and after ashing, at temperatures between 1250' and 1350°C. The specific gravity, expansion and compressive strength of the products were measured. The response of the refuse to bloat is related to the chemical composition of the ash to yield a glass of desirable viscosity and to the presence of a material which will form a gas in the appropriate temperature range. Carbonaceous material within the particle is a negative factor since after the glassy phase forms, oxygen cannot enter the mass thus inhibiting bloating. Precombustion of the refuse is also detrimental since it removes substances of gas-forming capability. The fraction sinking at 2.60 yielded an aggregate which had the lowest specific gravity, greatest expansion and greatest compressive strength. The purpose of this study was to seek and evaluate possible relationships between the composition of coal refuse, as expressed by washability data and factors affecting the production of a lightweight aggregate from refuse by bloating. The study was related to an intense program in the Department of Mineral Preparation at the Pennsyl- vania State University to study the possible elimination of air pollution from coal refuse fires by producing a low-carbon secondary refuse. Another phase of this program is considering possible uses of such a secondary refuse. Thus one study was to determine if a lightweight aggregate could be produced from this new refuse material and what effect the nature of refuse beneficiation would have upon the characteristics of a commercial aggregate product. It was hoped that these studies would assist in the design of a process and in establishing the optimum specific gravities at which refuse separation could be made in respect to the production of a low grade fuel from the float product and a raw material for lightweight aggregate from the sink product. The combination of producing a saleable low grade fuel and a lightweight aggregate, while at the same time minimizing disposal costs and air pollution contributions would be attractive to the coal mining industry. MECHANISM OF BLOATING Austin, Nunes and Sullivan,1 Ehlers,3 Everhart, 4 Riley7 and others, have stated that bloating is an expansion process in which two essential conditions exist simultaneously. These are: the development of a glassy phase over a relatively wide temperature range (the viscosity of this glassy phase plays a major role in the retention of the evolved gases) and the evolution of gases (SO2, SO3, CO2 and O2) from mineral decomposition in sufficient quantities at appropriate temperatures to form a cellular structure in the mass. Unless these two "type" reactions take place at the same time or in overlapping ranges of time and temperature, cellulation will not occur. In this event, the gas will escape or the melt will be too fluid to retain it; or if retained, the cells may be too large or the walls too thin for good strength in the product. The stages that occur when clays and shales are heated in an oxidizing atmosphere may be summarized as follows: 1) Drying and removal of free water to 200°C. 2) Absorbed water dehydration period (200 to 480°C). 3) Chemically-combined water dehydration period (480 to 700°C).

Jan 1, 1965

By D.E. Norquist, J. E. Moeller

The results of wear on marked balls, 4, 31/2, 3, and 2 in. diam are given. All balls were forged steel of practically the same chemical analysis and hardness. The results indicate that balls in a given mill for a given length of time will have equal diameter losses, regardless of size. IN order to determine the relative wear rates of several sizes of grinding balls, groups of 4, 31/2, 3, and 2 in. balls were marked individually and were charged, all at the same time, into each of two production mills grinding copper ore. The remainder, and vast majority, of the ball charge consisted of 2 in. diam, and smaller, white, cast iron balls. The original weight of each test ball was determined and recorded. Some of each group of test balls were recovered from the mills periodically, individually reidentified, and reweighed. The test balls were recovered during regular maintenance shutdowns, at approximately thirty-day intervals, so as to avoid disrupting operations. As soon as the weights had been recorded, each marked ball was recharged into the mill from which it had been taken. The test units were mechanically the same and theoretically received equal tonnages of feed. All of the test balls were of forged, alloy steel composition with only slight variations in chemistry that would not be expected to affect the physical properties. All were heat treated in the same manner to produce a high hardness, as equal as possible for all sizes and as uniform as possible from surface to center. Generally speaking, the hardness of the portion worn from the balls during the test ranged from 62 to 65 Rockwell C. The microstructure was, therefore, predominately martensitic. The method of marking the test balls consisted of forming a small, round hole, 3/16 or 1/4 in. diam, into the center of each test ball with a Thomas Metal Master disintegrator, which produces a hole in fully hardened steel without affecting the hardness of the surrounding metal. After the hole was formed, each test ball was individually weighed to the nearest gram and the weight was recorded. The balls were grouped as to size and each group assigned a code letter. The individual balls within the various groups were then assigned a number. A small copper disc was stenciled on one side with the group letter and on the other side with the individual ball number and dropped into the hole in the corresponding test ball. The hole was then plugged with a low-melting-point metal alloy, which could be melted out in boiling water. Half of the test balls in each group were charged into one mill and the other half into another mill, so that all test balls in each mill would be subject to, as nearly as possible, identical conditions for an equal length of time. Previous testing had indicated that the wear rates on balls of different sizes could not be accurately compared if weight loss, or percentage weight loss, were used as a basis for comparison. Fig. 1 is a graphic record of the average weight loss for each size group in mill No. 1, and it becomes readily apparent that the larger balls lose substantially more weight in a given length of time. Fig. 2 is a graphic record of the average percentage weight loss for each size group in mill No. 1, illustrating that the smaller balls definitely lose a greater percentage of their original weight in a given length of time. It was, therefore, decided to convert the actual weights of the test balls to diameter and follow the diameter losses periodically to see if the wear rates

Jan 1, 1951

By D. E. Norquist, J. E. Moeller

The results of wear on marked balls, 4, 31/2, 3, and 2 in. diam are given. All balls were forged steel of practically the same chemical analysis and hardness. The results indicate that balls in a given mill for a given length of time will have equal diameter losses, regardless of size. IN order to determine the relative wear rates of several sizes of grinding balls, groups of 4, 31/2, 3, and 2 in. balls were marked individually and were charged, all at the same time, into each of two production mills grinding copper ore. The remainder, and vast majority, of the ball charge consisted of 2 in. diam, and smaller, white, cast iron balls. The original weight of each test ball was determined and recorded. Some of each group of test balls were recovered from the mills periodically, individually reidentified, and reweighed. The test balls were recovered during regular maintenance shutdowns, at approximately thirty-day intervals, so as to avoid disrupting operations. As soon as the weights had been recorded, each marked ball was recharged into the mill from which it had been taken. The test units were mechanically the same and theoretically received equal tonnages of feed. All of the test balls were of forged, alloy steel composition with only slight variations in chemistry that would not be expected to affect the physical properties. All were heat treated in the same manner to produce a high hardness, as equal as possible for all sizes and as uniform as possible from surface to center. Generally speaking, the hardness of the portion worn from the balls during the test ranged from 62 to 65 Rockwell C. The microstructure was, therefore, predominately martensitic. The method of marking the test balls consisted of forming a small, round hole, 3/16 or 1/4 in. diam, into the center of each test ball with a Thomas Metal Master disintegrator, which produces a hole in fully hardened steel without affecting the hardness of the surrounding metal. After the hole was formed, each test ball was individually weighed to the nearest gram and the weight was recorded. The balls were grouped as to size and each group assigned a code letter. The individual balls within the various groups were then assigned a number. A small copper disc was stenciled on one side with the group letter and on the other side with the individual ball number and dropped into the hole in the corresponding test ball. The hole was then plugged with a low-melting-point metal alloy, which could be melted out in boiling water. Half of the test balls in each group were charged into one mill and the other half into another mill, so that all test balls in each mill would be subject to, as nearly as possible, identical conditions for an equal length of time. Previous testing had indicated that the wear rates on balls of different sizes could not be accurately compared if weight loss, or percentage weight loss, were used as a basis for comparison. Fig. 1 is a graphic record of the average weight loss for each size group in mill No. 1, and it becomes readily apparent that the larger balls lose substantially more weight in a given length of time. Fig. 2 is a graphic record of the average percentage weight loss for each size group in mill No. 1, illustrating that the smaller balls definitely lose a greater percentage of their original weight in a given length of time. It was, therefore, decided to convert the actual weights of the test balls to diameter and follow the diameter losses periodically to see if the wear rates

Jan 1, 1951

By E. P. Abrahamson

The effect of transition element binary solid solution additions upon the re crystallization temperature of nickel has been investigated. All additions raised the re crystallization temperature. Both the rate of change of re crystallization temperature with at. pet solute and the limit of initial linearity are found to correlate with the free atom ground state outer electron configuration of the solute element. A comparison of all of the correlations for the transition elements studied has yielded a set of empirical relations, which allows the prediction of the effect of dilute binary transition elements on the recrystallization temperature of other transition elements. The work of Abrahamson, et al.1-7 on dilute binary solution alloys indicated a correlation between the free atom ground state electron configuration of the solute and both the brittle-ductile transition and re-crystallization temperature. Further, it has been shown3,4 that the limit of initial linearity may also be correlated with the solute electron configuration. Since previous studies have dealt with bee and hexagonal base elements, this study is made to note what effect, if any, the fee base structure might have. Nickel also serves to give a solvent configuration which will allow the comparison of all of the transition element solvents. Olsen8 has studied the effect of some trace elements upon the recrystallization of nickel. He included only Ti, Zr, W, Mn, and Co of the transition elements. The differences in change of recrystallization temperature were attributed to the solute atom size and to the solubility of the solute in nickel. PROCEDURE All alloys were made using 99.9 + pet Ni with 0.003 C, 0.015 Fe, 0.007 0, and 0.0007 H. The solute elements were 99.9 + pet pure. According to the published binary phase diagrams9 and metallo-graphic examinations at X750, all solute elements were in solid solution. The alloys were arc melted and remelted four times in the form of cubic 200-g buttons under an argon atmosphere. They were then hot forged at 800oC to 0.750 in. diam, machined to 0.60 in., vacuum annealed for 1 hr at 700°c, swaged to 0.40 in. and annealed at 700oC for 1 hr in vacuum. The grain size was checked and found to be 77 * 20 grains per sq mm. The specimens were then swaged to 0.187 in., yielding 76 ± 1 pet cold work. All alloys were then chemically analyzed for the solute addition. The interstitial contents remained at the values of the starting material when checked on random alloy specimens. The swaged rod was cut into 8.25 in. lengths and heat treated in a gradient furnace for 1 hr. The gradient was maintained at 250" to 850°C over an eight inch length, recorded by twelve thermocouples. Control was ± 3oC, accomplished at the hot end. The recrystallization was determined metallo-graphically over the entire specimen. The criterion chosen was that point on the specimen showing the first recrystallized grain at a constant magnification, X200. Specimens were repeated, and the agreement was found to be generally ± 3oC.

Jan 1, 1962