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By Paul A. Beck, M. N. Parthasarathi

The vecrystallization texture. formed by selective growth of random nuclei in an 80 pct volled 99.997 pct A1 crystal of initial orientation mear (123) (41.21 was found to consist of components related to the single-component rolling texture by 40 deg. rota-tiows around [111]axes. The relative-volume fractiovz of the various recrystallization-texture componezts may be accouzted for 012 the basis of the Lou) mobility of twist boundaries, if it is assumed that the mobility of the tilt boundaries also varies with their orientation. Similar results with a, aluminum-alloy cystal of the (110) [112] orientation, containing iron, silicon, and zinc, show that these solute contents do not impair the effectivezess of the oriented growth mechanism of re cry s-tallization- texture formation. In a previous investigation1,2 it was found that a sharp recrystallization texture is formed as a result of the oriented growth of random artificial nuclei in an aluminum crystal rolled to 80 pct RA, on the (110) plane in the [ 112] direction. Four recrystallization-texture components were found to occur, with orientations corresponding to 40-deg rotations around [111 1 axes of the deformation texture. Reorientations of this type were already found in earlier work,3,4 where the presence of random nuclei could be reasonably assumed, but was not rigorously documented. The same orientation relationship was found also by Lucke and Liebmann, who actually measured the orientation dependence of boundary-migration rates in the recrystallization of A1 crystals slightly deformed in tension.5,6 The occurrence in the recrystallization texture of only four of the eight crystallographically equivalent orientations of the type referred to above remained unexplained,1,2 although it was clearly not a result of the absence of suitable nuclei. Recently Burgers7 suggested that this effect may be due to the aniso-tropy of boundary mobility observed2'6; it was found that the recrystallized grains of the 40-deg [111]-rotated type grow much faster in directions perpendicular to the [ 111] they have in common with the matrix than parallel to this direction, i.e., the tilt boundaries have much higher mobility than the twist boundaries. The four orientations corresponding to

Jan 1, 1962

By J. E. Pavlick, A. G. Guy

The total creep of tin alloys containing antimony in solid solution was observed to decrease with increase in antimony content. However, near the solubility limit an anomalous maximum in deformation was. found, in agreement with similiar observations by Bochvar. IT has long been recognized that alloys may deform more rapidly under stress if there is a tendency for a phase change or other structural change to occur simultaneously. However, the phenomena involved are complex and in some instances the opposite effect, strengthening, may result.' This area of research has not attracted much interest in the western world, and although Russian investigators have studied it for the past 15 years their work has not received due attention here. Recently diametrically opposing views on one aspect of this problem have been espoused by two Russian investigators, Kornilov and Bochvar. The question is this: in certain binary alloys tested in creep at the temperature where the solute is at the limit of solid solubility, does the incipient formation of the second phase strengthen or weaken the alloy? Korni-lov's arguments in favor of strengthening were presented at the 1954 Symposium at the National Physical Laboratory, =Creep and Fracture of Metals at High Temperatures.The most recent statement of Boch-var's theory of weakening is in Oding's new book on creep and rupture.3 Although Bochvar agrees that strengthening occurs in some alloy systems, he argues that in certain alloys an anomalous weakening is observed. However, the extensive work of Korni-lov's group on creep properties of alloy systems has not revealed any anomaly of this type, but instead has tended to refute Bochvar's theory. This clear-cut controversy offered a good opportunity for a simple experiment to resolve the problem. The experiment and its results supporting Bochvar are the subject of this paper. However, it will be helpful first to sketch the present status of the larger question of the effect of a phase change or other structural change on plastic deformation. PREVIOUS WORK One of the first researches in this area was by Pfei1,37 who investigated the creep resistance of an 80 Ni-20 Cr alloy containing varying amounts of titanium. He found that the resistance to creep increased rapidly as the solid solubility limit in the alloy at 775'c was approached and slightly exceeded. With further addition of titanium the creep resistance decreased, presumably because of precipitation effects. Bochvar's first work in this field was a study in 1945 of "superplasticity" in zinc alloys containing 15 to 25 pct Al.4 He found that alloys quenched from about 400 had anomalously low hardness when tested below this temperature. The following year, in a paper on the dependence of mechanical properties on the composition and structure of alloys,5 he extended some observations of Kurnakov to predict that at high temperatures of testing the hardness values for solid-solution alloys might be lower than those for the component metals. He also pointed out the influence of changes in solidus temperature in affecting curves of hardness vs composition, and he

Jan 1, 1962

By H. D. Mellom

The direction of the optic or "C" axis of a uniaxial metal crystal can be found with the metallurgical polarizing microscope by examining two planes of section on the crystal. Complete orientation of the crystal can be determined if a twin crystal is common to both surfaces of section. Examination of Uniaxial Metals in Polarized Light-Rotation of a uniaxial crystal surface, properly prepared,' shows four extinction positions 90 deg apart, provided that the surface is not close to a basal section. One of these two extinction directions corresponds with the projection of the optic axis on the surface of section. This direction can be found if the 'sign of the rotationr2 for the metal is known. To find the direction of the optic axis, the crystal is rotated on the stage 45 deg from an extinction position. With a crystal of negative sign, to produce extinction the analyser must be rotated towards the optic axial direction and vice versa. All sections, other than basal, of a uniaxial crystal have the same sign of rotation and, since there is no change in sign with wave length, white light can be used for these measurements. U the sign of the rotation is not known the presumed direction of the optic axis can be determined assuming a positive sign. A third section cut normal to the presumed optic axis will show basal extinction if the assumption is correct. It is convenient to use the edge between the two planes of section as a fiducial direction common to both surfaces. The optic axis can be related to this direction. If the above measurements are repeated on the other plane of section and the angle between the two section planes measured, stereographic projection can be used to determine the orientation of the crystal optic axis. Determination of Complete Orientation—The complete orientation of a uniaxial crystal can be determined provided that a twin crystal is common to both surfaces of section, and the twin law is known. The orientation of the twin crystal optic axis can be determined in the same way as for the main crystal

Jan 1, 1962

By Franklin J. Hill, Theodore D. Tiemann

Sized fractions of Wisconsin Gogebic taconite were reduced with hydrogen over the temperature range from 600° to 1000°C. In general, the degree and rate of reduction increase with temperature. Particle size has no observable effect except in the smaller fractions at 900°C and above, where reduction is impeded, possibly due to the siliceous nature of the ore. Gaseous diffusion appears to be significant as a rate controlling factor at certain stages. THE depletion of high grade iron ore reserves in the United States has established the need to utilize all available iron ore deposits, both in long range planning and from the viewpoint of national emergency. This has led to extensive research and development in this field. The beneficiation of Wisconsin Gogebic taconite ore has been previously studied by investigators at the University of Wiscconsin, 1 the United States Bureau of Mines,, Battelle Memorial Institute, 3 and others. Methods investigated have included concentration by flotation processes, magnetic and gravity separation, magnetic roasting and various combinations of them. The foregoing studies have been concerned with the production of an enriched ore suitable for blast furnace use. If the ore could first be reduced to metallic iron and then beneficiated, the product could be used directly in the open hearth or electric steel-making furnace. The by-passing of the blast furnace should enhance the economic feasibility of the beneficiating process. The work reported here,4 was undertaken to establish data on the hydrogen reduction of Wisconsin taconite that would eventually lead to the development of an economic direct reduction process for this and perhaps other low grade siliceous ores. The volume of work on direct reduction can be judged by the fact that 240 direct reduction processes were patented in the United States alone up to 1951, 5 and numerous additional processes have since been developed. Some of the factors contributing to direct reduction development are: 1) The increasing capital cost of the blast furnace and its accessory equipment. 2) The decreasing availability of high grade domestic ore. 3) The high cost of steel scrap for use in the open hearth and electric furnaces. In general, direct reduction processes can be divided into two types; those using a solid reductant (coal, peat, lignite) usually carried out in a kiln, and those using a gaseous reductant (H2, CO) in a shaft furnace or a fluidized bed retort. As there is no low cost coal readily available in northern Wisconsin but natural gas could be quite easily obtained, it is believed a gaseous reductant process would offer the greater feasibility for use on Wisconsin taconite. It is hoped that this preliminary work will beof interest to other investigators in this increasingly important field. TACONITE ORE The ore used in the investigation was obtained originally from the U. S. Bureau of Mines, and consisted of a representative composite made up from trench samples of the Norrie, Pabst, Plymouth, Pence, and Yale members of the Wisconsin Gogebic range iron formation. Chemically, the ore contains approximately 52 pct SiO, and 30 pct Fe. X-ray diffraction and other studies indicate the principal minerals to be quartz (SiO2), hematite (Fe2O3), and goethite (Fe2O3. H2O). Minor amounts of iron containing silicates, siderite (FecO3), and magnetite (FeO-Fe2O3) are present. The iron minerals and quartz are so finely disseminated that the ore requires grinding to less than 200 mesh (74 µ) for essential liberation.l,2 The iron content of each of the several size fractions studied is shown in Table I. EXPERIMENTAL METHOD The method used throughout the investigation was based on that developed by the U. S. Bureau of Mines in Minneaopolis6,7 in which the course of reduction is followed by the loss in weight of the ore sample. More specifically, a 100-g sample of the size frac-

Jan 1, 1962

By H. W. Meyer, H. N. Lander, F. D. Delve

A method of calculating the changes in blast-furnace performance brought about by burden and/or blast modifications is presented. Essentially the method consists of three simultaneous equutions derived from materials and heat balances. These equations can be used not only to evaluate quantitatively the effect of changes in process operating variables on furnace performance, but also to provide a useful means of evaluating changes in process variables which cannot be measured directly. It has been customary for a number of years to use simple heat and materials balances as a basis for assessing blast-furnace practice. A good example of the method used to set up these balances is that proposed by Joseph and Neustatter.1 This approach to process assessment has limited utility, however, in that it cannot be used to predict the furnace coke rate or production under new operating conditions. Using an approach based on multiple correlation of blast-furnace variables, R V. Flint2 has developed an equation which may be used to predict the change in coke rate that will result from some changes in operating conditions with a reasonable degree of accuracy. Although this equation has useful applications in production planning, it cannot be used to study the relationships between the operating variables and the fundamental thermochemi-cal characteristics of the process. In attempting to analyze the blast-furnace process quantitatively, the idea of dividing the furnace into zones3 may at first appear attractive. In our present state of knowledge, however, it is not possible to define with any accuracy the physical limits of such zones in relationship to their temperatures or to the reactions which may occur in them. Although its application is restricted, the zonal approach to blast-furnace analysis is useful in some instances. For example, the change in the calculated flame temperature in the "combustion zone" caused by injecting steam constitutes information which is helpful in understanding why the addition of steam to the blast is best accompanied by an increase in blast temperature. The zonal approach cannot, at the present time, be used to establish the relationships between process variables and process performance if the whole process rather than part of it is to be considered. One of the earliest approaches to the problem of relating blast-furnace operating variables to pro- duction and coke rate was that developed by Marshall.4 Essentially Marshall's work showed that it was possible to estimate the performance of a furnace by solving three simultaneous equations which consisted of rudimentary carbon and heat balances plus a further equation relating the production, wind rate, and the carbon burned at the tuyeres. Although these equations did not include all of the chemical and thermal variables of the process, their derivation and application seems to be the earliest attempt which achieved any success in relating prior furnace operating data to the calculation of furnace performance under different blast conditions. Work carried out in Germany has been directed mainly towards prediction of coke rates using material and thermal balances rather than statistical methods. wesemann5 used prior furnace operating data as part of the basis for predicting the change in coke rate accompanying a change in burden composition. This author employed a method of successive approximations to estimate the secondary changes in slag volume and stone rate brought about by the change in coke rate. The most recent analysis, which seems to have been developed concurrently with the thermochemical model presented in this paper, has been described by Georgen.6 This author has succeeded in improving on Wesemann's approach by expressing the total changes in the slag volume and stone rate in terms of the change in coke rate itself. This is accomplished in a manner similar to that used in the thermochemical model described in this paper. Although Georgen makes use of a calculated furnace heat loss, he does not relate the heat loss per unit of hot metal to the production rate as is done in the present work. Georgen's approach may be used to calculate the changes in materials requirements accompanying changes in furnace operation; it cannot be used to assess the resulting changes in production. The fact that blast-furnace behavior can be interpreted by consideration of the heat requirements of the process was demonstrated by Dancy, Sadler, and Lander.7 In the analysis of blast-furnace operation with oxygen and steam injection these authors showed that it was possible to account for the changes in production and coke rate

Jan 1, 1962

By Hsun Hu

The formation of annealing textures in high-purity silver, from the various rolling textures obtanled in the course of texture transition, was studied. It was found that from a brass-type rolling texture the recrystallization texture is mainly (120) [211] type, which is quite different from the recrystallization texture of brass. From a predominantly copper-type rolling texture, the reclystallization texture is mainly (100) [001]. The recrystallization texture of silver- varies also with the degree of purity. In each case, however, the reorientation can be expressed as [Ill] rotations of 30° to 40°, which is consistent with the oriented growth theory of the formation of annealing textures. ThE recrystallization textures of rolled silver were studied long ago by Glocker and co-workers (1924-27) and were reported to be (113) [iil] upon annealing at low temperatures.1 Since that time, no further study of the recrystallization textures of silver, particularly with the modern techniques of quantitative texture determinations, has been reported in the literature. In a previous study2y3 it was found that the rolling texture of high-purity silver (99.999 +pct pure) is changed gradually from the common silver- or brass-type to the copper-type by raising the temperature of rolling from 0" to 200°C. The formation of annealing textures from the various rolling textures in the same material is, therefore, of considerable interest. The present paper constitutes the results of such a study. MATERIAL AND METHOD Specimens were taken from the same strips of high-purity silver* that were used previously for

Jan 1, 1962

By J. R. Lucas, H. E. Rutherford

The primary objective of this research was to evaluate the feasibility of ultrasonic testing for the purpose of analyzing the structure and properties of rock material. A secondary objective of this study was to determine experimentally the elastic wnstants of various rock specimens with the use of ultrasonic equipment. Elastic constants can definitely be determined quickly and accurately by ultrasonic investigation. With proper equipment there are indications that ultrasonic waves could be utilized in the detection of flaws, such as fractures and planes of weakness, measurement of thickness, and the study of structure of rock material. Ultrasonic principles have been applied in many industries for the purpose of determining the structural characteristics of various materials. The principal applications of interest here are detecting flaws, measuring thicknesses, and determining elastic constants. The main advantage of ultrasonic analysis is that it is nondestructive. It also has extreme sensitivity, high penetrability, good accuracy, rapid response, and the necessity to have access to only one side of the specimen. These various applications and advantages lead one to think that ultrasonic principles might be applied to rock material in situ for purposes of analyzing its structural characteristics. Therefore, the primary objective of this research was to evaluate the feasibility of ultrasonic testing for the purpose of analyzing the structure and properties of rock material. A secondary objective of this research was to determine experimentally the elastic constants of various rock specimens with the use of ultrasonic equipment. The term ultrasonics is given to that branch of acoustics dealing with periodic sounds whose fre- quencies are above the audible range or above approximately 15,.000 to 20,000 cps. The first practical production of this high frequency sound was made possible after World War I due to developments of electronically controlled sound wave sources. At the present, the maximum practically attainable ultrasonic frequency is approximately 1000 megacycles per sec. Sound waves of sufficiently high frequency can be made to travel in a beam with little spreading. Therefore, such a beam can explore a material and detect nonhomogeneities in it by reflection. This is the principle of the ultrasonic reflectoscope invented by F. A. Firestone' in 1942. An ultrasonic beam, on pulse-penetratink a solid material medium, produces an echo when it strikes a flaw which has different acoustical properties than the surrounding medium. This echo can be detected by the same transducer which sends out the original pulse. This principle is the basis of the important industrial techniques of nondestructive ultrasonic testing of metals and other solid material. Later developments in the field of ultrasonic testing of solid material have been mostly improvements in equipment and instrumentation. To date, most of the industrial applications of ultrasonic analysis of solid bodies have been in the aircraft, electrical, and nuclear energy fields on the nondestructive testing of metal. The one solid material similar somewhat to rock material, upon which some work has been done to apply ultrasonic testing techniques to study structural integrity, is concrete. Jones and Gatfield3 briefly summarize this work on concrete. Their basic conclusion was that the strength of concrete was a function of the change of the longitudinal sound wave velocity in the concrete. Only recently has any extensive study been made to apply ultrasonic testing techniques to rock material. Lutsch studied rock material by an ultrasonic pulse method to determine the extent and degree of fracture of rock faces. Lutsch states that the number of observed reflections is a measure of the degree of fracture and that only ultrasonic waves are able to detect fractured zones subjected to high pressure. Suzuki, Sasaki, and Siohara5 studied the characteristics of the sonic wave in rock for propagation over a wide range of wave lengths. They indicated that, in rock, the propagation constant and attenuation of the

Jan 1, 1962

By Pierre R. Hines

The first progress in American ore dressing practice was made in the mills of the Mother Lode in Calif., the Comstock Lode in Nev., and Gilpin County in Colo., during the years 1861 to 1870, when the ancient wooden stamp battery, with square wooden stems, was converted into the 'California' stamp made of wrought and cast iron, with round stems which rotated. Eli Whitney Blake invented the jaw crusher in 1858 for stone crushing, and it was soon used for crushing ore. F. W. Gates' gyratory crusher followed twenty years later. S. R. Krom, Thomas A. Edison, and others improved the Cornish rolls by increasing their size and spring pressures; the Symons Brothers made horizontal and vertical disc crushers; W. Ball and E. T. Leavitt designed powerful steam stamps for Lake Superior native copper ores; and jigs were mechanized. William B. Frue, a mill superintendent in the Lake Superior copper district, invented the vanner in 1874. Arthur F. Wilfley built his riffled concentrating table in 1895, just after Dr. Robert H. Richards commenced his Ore Dressing. The Wilfley table so changed concentrator flow sheets that Dr. Richards was compelled to revise his text, and its publication was delayed until 1903. The value of sizing or classifying before concentration was recognized. Dr. Richards had persuaded the Anaconda Copper Mining Co. to install round tables with special surfaces to catch the 'extremely fine free mineral.'l Gravity concentration had achieved almost every refinement for recovering or separating minerals by the difference in their specific gravities. However, one serious problem remained unsolved, i.e., how to retrieve the enormous loss of the extremely fine mineral in the slime portion of the ore. Slime, then, as now, was not a precise term due to the variation in the mineral composition of the ores and the different requirements in crushing, grinding, sizing, and classifying. At that time, slime was considered to be fine sand and colloidal material passing 100 mesh.2 Most sulfide ore minerals are more friable than their associated gangue minerals, so that crushing and grinding increased the proportion of the extremely fine ore minerals in the slime. Sparkling specks of galena, chalcopyrite, argentite, or ruby silvers, according to the ore, floating away on the tailing stream from vanners and slime tables, were familiar sights in the old gravity concentrators. Gravity concentration practice was aimed at recovering the ore minerals at the coarsest possible size because the recovery was higher and unnecessary

Jan 1, 1962

By J. M. Dahl, R. J. Warrick, O. K. Riegger, H. Van Vlack

A liquid which is rich in oxygen (and silicon) develops at steel rolling temperatures in resulfurized and plain-carbon steels. This liquid fluxes solid manganese sulfide. The composition of the liquid and the resulting microstructures vary with the manganese/silicon/oxygen ratios in the steel. The observations and conclusions zuhich are presented are used 1) to suggest a mechanism for MnS deformation in resulfurized steels, and 2) to rationulize hot-shortness anomalies between plain-carbon and resulfurized steels. 1 HIS is a summary of the dependence of sulfide inclusion microstructures upon steel composition, and an interpretation of the behavior of sulfide inclusions at steel-rolling temperatures. Sulfide inclusions are known to have several metallurgical effects upon steel. Their effects upon hot-shortness are best appreciated. Although hot-shortness is well known, it is questionable whether its mechanism is fully understood because there are several anomalies in our interpretation. For example, why should not high sulfur contents produce extensive hot-shortness in free-machining steels ? A second metallurgical consequence of sulfide inclusions appears because sulfide inclusions improve machinability. Furthermore, globular inclu- sions are to be desired over elongated inclusions. To date, we know that lower silicon contents (< 0.010 pct) favor the globular sulfides, but we do not know why this interrelationship between silicon content and inclusion shape exists. Finally, the evidence is strong that the surface quality of a hot-rolled steel is particularly sensitive to the sulfur content. SUMMARY OF PREVIOUS WORK The role of sulfur in hot-shortness was first suggested during the past century. It is uncertain who was the first to conclude that sulfur was less deleterious in the presence of manganese, and that manganese altered the sulfide phase from a liquid FeS to a solid MnS at steel-rolling temperatures. However, Urban and chipman&apos; emphasized that liquid FeS may accumulate as an interdendritic film during solidification. More recently, Keh and Van lack&apos; showed that the intergranular liquid does not completely surround the metal grains at all rolling temperatures. Rather, a small finite dihedral angle exists when geometric equilibration is attained at

Jan 1, 1962

By A. J. Jacobs, G. Katz

MANY of the studies of intermetallic compounds containing uranium were performed during the early 1940&apos;s under the aegis of the Manhattan Project. Subsequently, much of this work was declassified and published after 1949. In some instances this early work, completed with relatively impure materials, represents the only source of X-ray diffraction powder data available in the literature. In the case of the intermetallic compound U,Fe some discrepancies in the powder pattern exist in the literature. Since this compound has been prepared in this laboratory, it is believed that the publication of the indexed powder pattern would help clarify the conflict in the literature. In studies of the U-Fe system, Gordon and Kauf-mannl and Grogan and Clews2 independently reported the intermetallic compound U,Fe in 1950. The crystal structure was described by Baenziger, Rundle, Snow, and Wilson3 in 1950. It is isostructural with U,Mn, U,Ni, and U,Co and crystallizes in a body-centered tetragonal lattice. The lattice constants determined by Baenziger et al. are: giving an X-ray density = 17.7 g cm-3 for 4 mol per unit cell. The compound used in this study was prepared by melting a stoichiometric mixture of the constituent metals in an argon-arc furnace using a nonconsum-mable tungsten electrode. Before the argon of 99.98 pct purity was introduced into the furnace, it was passed through CaC1, to remove water vapor and afterwards through a stainless steel tube containing calcium turnings heated at 600°C for the removal of nitrogen and oxygen. The purity of the uranium used was better than 99.9 pct and that of the iron was 99.97 pct. Before and during melting a zirconium getter was used to further purify the argon atmos-

Jan 1, 1962

By A. L. Mular

lnput energy-size modulus relation at small reduc-tion ratios is expressed by Et = (M, -Mt) k;. In some cases 13 is close to Schuhmann&apos;s distribution modulus a in value. Experimental results in conjunc-tion with the equation demonstrate the fact that energy input which produced fracture is not expended on unbroken starting material inside the mill at any time. Recently, schuhmann1 derived the Charles equation2 using the postulate that complex com-minution operations can be considered as a summa- tion of many comminution events. The fragments resulting from each event are assumed to follow the Gaudin-Schuhmamn distribution. In his derivation, Schuhmann implies that the size distribution of the total mass of a material is determined by the fraction of that mass actually subjected to comminution. Consider a feed to contain a volume, Vo, of uni- formly sized homogeneous material. After t seconds of grinding, let the volume of broken material be Vo - Vt where Vt is the volume of starting material not yet broken. The size distribution of the broken material is given by: where V is the cumulative volume less than size X, and k, is the size modulus of the broken material at time t. The distribution for the total volume at this

Jan 1, 1962

By J. A. Cahill, A. D. Kirshenbaum

Using an alumina or zirconia crucible with an alumina sinker or a molybdenum sinker coated with zirconium dioxide, the density of liquid iron was determined by the immersed-sinker method over the temperature range of 1800" to 2500°K. The density, with respect to temperature, is ex-Dressed by the equation Dg/cm = 8.523 - 8.358 X 10 T&apos;K The molar Volumes and thermal coefficients of expansion were calculated. Iron, upon me1ting, was found to expand 3.5 pct. A basic knowledge of the physical properties of materials at high temperatures is becoming increasingly important. A check of the literature shows, that in spite of the importance of iron, very few measurements have been made of its physical properties in the liquid state. Density measurements have been made by Benedicks and his collaborators1g using the method of balanced columns, by Desch and smith4 using the immersed sinker method with an alumina sinker, by Lucas using the maximum bubble method5 and by Stott and endall&apos; who used an alumina pyknometer. In the method of balanced columns, the difference in level of molten iron in two arms of a U-tube, together with the corresponding difference of pressure had to be measured. The formation of gas bubbles in one or both arms was a great source of error. These values are very erratic. They vary from 6.83 to 7.45 g per cm3 at the melting point (1805"~) and from 6.45 to 7.15 g per cm3 at 1890°K. Stott and Rendall determined the density at 1837"K, with a reproducibility of *0.2 pct. They used an alumina pyknometer fired to 1973°K. The vessel was filled in a vacuum furnace by immersion in the liquid metal. When thermal equilibrium was attained, the pyknometer was withdrawn, cooled, the ingot removed and then weighed. The chief disadvantage of the method was the difficulty of inserting the pyknometer without cracking it. The authors have been able to determine the density of liquid iron from its melting point up to 2500°K, by using the immersed-sinker method, with A1203 or ZrOz crucibles and A1203 or molybdenum sinkers coated with Zr02, Fig. 1. EXPERIMENTAL Apparatus. In these studies the source of heat was the carbon tube resistance furnace with an argon atmosphere described previously.7 Experimental runs were made using either Ala3 or ZrOz crucibles. The sinkers used were 1) pure A1a3 and 2) molybdenum coated with ZrOz. The crucible, 2 1/8 in. in diam and 3 in. high, was centered in the furnace on an Ala3 of Zr02 pedestal. The sinker, 1/2 in. in diam and 1 1/2 in. long, together with a counter weight, was suspended from an analytical balance into the melt by a molybdenum wire. Procedure. The procedure, as described previously,&apos; consisted in measuring the weight loss of the sinker in the liquid iron while determining simultaneously the liquid iron temperature by means

Jan 1, 1962

By R. L. Brown, E. A. Swanson

THE Buchans ore bodies are located in central Newfoundland, three miles north of Red Indian lake. The townsite of Buchans was named after a Royal Navy Captain who, while attempting to make contact with the Beothuck Indians, camped in the area in 1820. Ore was first found at Buchans by a Mic Mac Indian, Matty Mitchell, who discovered one of the three small orebodies in the bed of the Buchans river. The Anglo-Newfoundland Development Company, which holds mineral rights in the area, developed the orebody, but was forced to give up the venture because of difficulties encountered in separating the various sulphides. The American Smelting and Re-fining Company developed a flotation process which was capable of economically separating and concentrating the various sulphides, and, in 1926, they took a long-term lease on the property.

Jan 1, 1962

By R. J. Wasilewski

Axial expansion has been determined by X-ray diffraction up to 600° to 760°C in a titanium and four high-oxygen alloys. Expansion data cannot be fitted to the usual quadratic expression and anomalies observed are believed indicative of the changes in the bonding configuration of the valence electrons. Furthermore, there is significant disagreement between data obtained on poly crystalline and single crystal powder specimens. The major disagreement occurs within the temperature range (-470°C) where both mechanical and electrical properties also show markedly anomalous behavior. X. HIS work forms part of an investigation of physical properties of pure titanium and its osolid solutiono alloys with oxygen and nitrogen. In view of the anomalies observed in both the electrical resistivity&apos; and the susceptibility behavior it was decided accurately to determine the thermal expansion behavior of the pure and alloyed a titanium. PREVIOUS WORK The axial expansion coefficients reported for pure titanium are listed below. As can be seen, there is a marked discrepancy between the axial expansion and the experimentally determined coefficients on poly crystal line material. Thus, if we take the most recently reported axial expansivities3,4 we obtain perature interval of 25o to 700°C. The experimental value reported for polycrystalline metal is, however, of the order of 9.7 x 10o6 per OC. EXPERIMENTAL I) Pure Titanium. High purity titanium powder of -325 mesh was used throughout most of this work. The only significant impurities present were the interstitials, oxygen and nitrogen, which analyzed respectively 650 and 80 ppm. The purity of the ma-

Jan 1, 1962

By C. H. Li, R. J. Stokes, T. L. Johnston

A portion of the Ni3Cr-Ni3Al phase dzagram has been investigated, including the precipitation of 1 (Ni3Al) as well as the existence of ordered Y (Ni matrix), Extensive metallographic studies by electron microscopy have been carried out and X-ray diffraction diagrams have been taken at both elevated and ambient temperatures, No long-range ordering of the phase was found above 893°C (1639°F) in the compositional range investigated. The high rate of formation of the ordered ?1 phase upon quenching has been confirmed, a phenomenon which up to the present Lime has retarded the understanding of this phase diagram, Specimens with controlled amounts of ?1 exhibited up to a six-fold improvement in yield and creep strength compared with single-phase Ni-Cv-A1 alloys. MOST of the important high nickel heat-resistant alloys are related to the nickel-chromium-aluminum system. One of the important functions of the aluminum, often accompanied by titanium, is to produce a precipitate of the very fine ?1 phase (Ni3A1, X) where X may be Ti, Cr, or other elements. A number of investigators1-" have demonstrate the presence of y&apos; in these alloys but most of their materials contained large amounts of other elements resulting in appreciable amounts of con- fusing phases such as carbides. Further clouding of the precise role of y&apos; has been the suspected existence of an ordering reaction in the y matrix itself, ro-3,12-17 It appeared from these investigations that aluminum in Ni-Cr alloys would raise the ordering temperature of the matrix from 540°C at NisCr to 1300°C at Ni,Al. In support of this possibility, the matrix phase in the parallel Ni-Fe-A1 system is ordered to very high temperatures.1 OBJECTIVES OF THIS RESEARCH From this survey of the literature it appeared desirable to conduct an investigation of the simple Ni-Cr-A1 system using the alloys of the highest available purity to avoid the complication of foreign phases and thereby isolate the structures in the Ni-Cr-A1 system. Procedures were developed to study ? - ?o and ? - ?1 equilibria. Preliminary mechanical tests at elevated temperatures were also conducted.

Jan 1, 1962

By R. S. Olson

The operation of a series wash thickener-two stage filtration circuit determines the soluble loss in many hydrometallurgical operations A study of this circuit yielded expressions which permit calculation of soluble loss for almost any condition of operation. The soluble loss over a range of the circuit variables is presented to illustrate and evaluate circuit performance, The interrelation of factors affecting filter performance and some of the wash circuit, variables are quantatively described. Filter wash, which is governed by wash zone size, filter pulp level and filter feed pulp density, has the greatest affect on soluble loss. Excepting clothing blinding and flocculation the factors which decrease filter capacity also decrease soluble loss. Repulping with water, under some circumstances, can bean important means of soluble loss reduction. Water for primary filter wash, leach pulp density repulp density and wash thickener underflow density have little effect on soluble loss. The dilution of both o the filter pulps with wash solutions is suggested as a means of reducing soluble loss, and at the same, time, controlling the performance of the filters. Blowback and filter cloth blinding seriously increase soluble loss.

Jan 1, 1962

By F. R. Brotzen, J. Taranto

SEVERAL investigators have computed stacking-fault concentrations from X-ray diffraction data.&apos;-&apos; The method generally employed relates the line shift to the stacking-fault probability. In this investigation platinum filings of 99.99 pct purity screened to -325 mesh were studied after having been subjected to various annealing treatments. The lines were measured on a General Electric XRD-5 spectrogoniometer using CuK, radiation. The centroid of the broad reflections was determined by the method proposed by pike.&apos; The stacking-fault probability was calculated by the formula given by Warren and warekois,3 with the assumption that all stacking faults were on the (111). Various high-angle reflections were used, but most data collected refer to the shift in the (400) reflections. When the filed platinum powder was annealed at 1200°C for 20 min the stacking fault concentration was too small to be detected. The stacking-fault probability in freshly filed specimens, as determined by the line shift relative to the annealed specimen, was about 0.016, Fig. 1. If the faults would be created only by extended dislocations, the dislocation density in the filed specimen would be about 3X1012 cm-2. The average stacking-fault width of about 21 which was used in this computation, is that given by Thornton and Hirsch.7 The mechanism by which stacking faults are annihilated during annealing is not yet fully understood. The isothermal results obtained do not seem to support the simple hypothesis of a first-order decay. On the other hand, the analysis by Kuhlmann, Masing, and Raffelsieper8 for the loss of dislocations during recovery agrees much better with the experimental data of this investigation. This analysis yields an activation energy of 29 ± 8 kcal per mol for the disappearance of stacking faults in cold-worked platinum during annealing. Even if one takes into account the lack of accuracy inherent in this X-ray method, the activation energy found is substantially less than that of self-diffusion in platinum, i.e., 61.6 kcal per mol.9 The results therefore suggest that processes other than dislocation climb, which involves the activation energy of self-diffusion, are responsible for the loss of stacking faults in platinum during annealing. The broad reflection lines became sharper early in the recovery process, Fig. 1. The sharpening occurred well before the stage during which stacking faults disappear. This lends support to Nowick&apos;s10

Jan 1, 1962

By E. P. Abrahamson II

The effect of transition element binary solid-solution additions upon the recrystallization temperature of vanadium has been investigated. Cr, Fe, Co, Ni, Mo, Ru, Rh, Os, and IY lower the recrystallization temperature, while Ti, Mn, Zr, Cb, Pd, Hf, Ta, W, Re, and Pt raise it. The majority of elements have their greatest effect in less than 0.15 at. pet. Both the rate of change of recrystallization temperature with atomic percent solute and the limit of initial linearity are found to Correlate with the free atom grozdnd state outer electron configuration of the sollte element. THE work of Abrahamson and Grant1 and Abraham-son and Blakeney2 has shown that the solute&apos;s elec- tron configuration appears to be a prime determinant of both brittle-to-ductile transition and recrystallization temperature in dilute binary alloys. It has also been shown by Abrahamson3 that the limit of linearity, i.e., the limit of initial linear change of recrystallization temperature with atomic percent solute, is also a function of the electron configuration of the solute in iron base alloys. Because of the systematic nature of the solute electron configuration correlation, it is to be expected that some systematic variation might be observed upon changing the solvent. Thus, this study of recrystallization in vanadium base alloys is the first of a series aimed at defining the role played by the electron configuration of solute in determining the recrystallization characteristics of dilute transitional alloys. PROCEDURE All alloys were made using 99.8 pct V containing 0.011 C, 0.024 N, 0.08 0, 0.006 H, 0.035 Ta, and

Jan 1, 1962

By H. R. Gardner

The heat treatmmt of plutonium was studied using the Jominy end-quenching technique commonly used for determining the hardenability of steel. Plutonium specimens were end-guenched from temperatures in each of the ß, y, d, d&apos;) and E phases. One series of specimens with a low-iron content, 165 pprn Fe, and another gvoup with a high-iron content, 678 pprn Fe, were used in order to study the effect of a Pu-Pu,Fe eutectic network on the hardness and micro-structure. Hardness traverses indicated no significant variations in hardness with either cooling rate or quench temperature. Metallographic studies indicated major effects on microstructure. Grain size was found to vary markedly with quenching temperature and cooling rate. It was determined that the Pu-PueFe eutectic network could be modified extensively by heat treatment, including spheroi -dization in the y phase and 6 phase below 413°C. An unidentified spheroidal inclusion was observed to go into solution in the delta and higher temperature phases. 1 HE element plutonium is unique among metals in that it has six allotropic forms in the solid state.&apos; These have been designated&apos; as the a, ß, y, d, d&apos;, and phases. The respective phase transformations occur at approximate temperatures of 122", 210°, 319°, 450°, and 480°C with a melting point at 640°C. With this number of phase transformations it becomes pertinent to consider the effect of heat treatment and cooling rate in the various phases on the microstructure and hardness of plutonium. To determine; the effect of a wide range of cooling rates, the Jominy end-quenching technique was applied to cylindrical plutonium specimens. In addition, since the presence of iron in amounts greater than 500 pprn is common in plutonium and results in a network of the Pu-Pu6Fe eutectic, it was decided to study heat treatment effects on two bomb reduced plutonium buttons with different iron contents. A low iron button containing 165 ppm Fe and a high iron button containing 678 ppm Fe were selected for this comparison. EXPERIMENTAL PROCEDURE Experimental Material. The cylindrical bars for Jominy quenching were cast from button stock in vacuo in MgO coated graphite molds. Metal pouring temperature was approximately 950°C and the molds were preheated to 300°C. The castings were machined to 0.5 in. diam. by 2.5 in. long cylinders. Chemical analysis and density data for the two groups of Jominy specimens containing different iron contents are presented in Table I. Except for iron, heats 19-12-1 and 20-2-1 are comparable within the limits of analytical accuracy. Representative specimens from the low-iron and high-iron bars were taken for metallographic examination. The low iron specimen was found to have extensive microcracking, Fig. 1. In addition, numerous unidentified spheroidal inclusions were present, Fig. 17. The average grain size of the low-iron plutonium is 0.068 mm, Fig. 4. In the high-iron plutonium, a Pu-Pu6Fe eutectic network is prominent, Fig. 7. The average size of the network is 0.100 mm. Unidentified spheroidal inclusions were also common in the high-iron plutonium. The average grain size of the high-iron plutonium is 0.036 mm. Experimental Technique. A Jominy end-quenching fixture was fabricated for glove box use. A 2.5 in. water height was used with an orifice of 0.250 in. ID. The orifice to specimen distance was maintained at 0.5 in. Annealing temperatures of 160°, 265°, 400°, 465°, and 535°c were chosen for the study of the effect of quenching from ß, y, d, d&apos;, and e phases on microstructure and hardness. During quenching, cooling curves were obtained from the Jominy specimens at distances from the quenched end of 1/16, 1/8, 3/8, 3/4, 1-1/4, and 2 in. Cooling rate calculations were made from the cooling curves for temperature intervals of 100° to 110° 160" to 170°, 330" to 340°, 420° to 430°, and 490° to 500°c. These temperature intervals were chosen

Jan 1, 1962

By W. M. Albrecht, W. D. Klopp, R. I. Jaffee, B. G. Koehl

Kinetic studies were made of the reactions of tantalum with oxygen, nitrogen, and air at 400o to 1500°C. The tantalum-oxygen reaction is linear from 500° to 1250°C. The tantalum-nitrogen reaction follows a cubic rate law at 400° to 700°C and a parabolic rate law at 800" to 1475°C. The reaction behavior in air is initially parabolic followed by a transition to linear behavior. In the search for high-temperature materials, considerable interest is being shown in the refractory metal, tantalum. It is the third highest melting metal with a melting point of 2996°C. Also, tantalum has excellent ductility, making it one of the most workable refractory metals. In considering high-temperature applications of tantalum, the oxidation kinetics of the metal must be known. Such information also serves as a basis for the development of corrosion resistant tantalum-base alloys. Therefore, this study was made to investigate the reaction of tantalum with air, nitrogen, and oxygen. LITERATURE Several oxides of tantalum have been reported. The pentoxide, Taz05, is the only oxide of tantalum whose identity has been established. A high-temperature modification, aTa2Os, has been reported by several investigators.1-4 A low-temperature phase, ßTa2O5, undergoes an allotropic transformation at 1320o to 1350oC. 5-8 Four other oxides of tantalum have been reported. The oxides TaO2, TaO, and Ta4O have been reported by schonberg.9 A suboxide Ta2O, was observed by Wasilewski 6. However, the presence of oxides lower than Ta2O5 is questioned by Lagergren and Magneli.7 In oxidation studies, vermilyeal0 and Peterson, et al.,12 reported one possible phase intermediate between Ta and Ta2O5. Only Ta2O5 was formed in the tantalum air reaction, as reported by Michae1.l3 Several studies have been made on the kinetics of the tantalum-oxygen reaction. vermilyeal4 investigated the range 50° to 300°C and found that the rate of growth of a thin adherent oxide film could be described by the Cabrera-Mott theory. Gulbransen and Andrew15,18 studied the reaction kinetics of tantalum in oxygen pressure of 1/10 atm at 250° to 450°C. At all temperatures the reaction followed the parabolic rate law for periods up to two hours. The oxidation behavior in the range 500" to 1000°C was found to be linear at oxygen pressures of 0.2 to 600 psi according to Peterson. et al.l1 At very low pressures (1 x 10-3 to 2 X lo-&apos; mm of Hg) Gebhardt and seghezzi17 reported linear oxidation at 800° to 1500°C. The reaction of tantalum with air is similar to the reaction with oxygen. Studies have been made by Waber, et a1.,12 and Michae1.l3 Two nitrides of tantalum, TaN and Ta2N are known. Their structures have been determined by Brauer and Zapp 18,19 The tantalum-nitrogen reaction kinetics have been investigated by Gulbransen and Andrews. 15, 16 The reaction follows the parabolic rate law at 500° to 850°C at a nitrogen pressure of 1/10 ,atm. At the same temperature, the tantalum-nitrogen reaction is much slower than the tantalum-oxygen reaction. EXPERIMENTAL TECHNIQUES Material— The material used in this study was high-purity, electron-beam-melted tantalum obtained from the Temescal Metallurgical Corp. The hardness of the as received ingot was 76 Vhn. The analysis of the material is given in Table I. Methods—Cylindrical specimens of tantalum approximately 0.9 cm in diam and 0.5 cm in length

Jan 1, 1962