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By D. Coutsouradis, L. Habraken, P. Nicolaides

The TTT curves of 0.1 pct C, 13 pct Cr steels containing up to 12 pct Co have been determined in order to establish whether the effect of cobalt is similar to that observed m plain carbon steels. It is shown that cobalt increases the incubation time and decreases the transformation rate, though not in an uniform way. The bainitic transfornation is displaced to lower temperature and overlaps partially the martensitic zone. ThE effect of cobalt on the transformation of a plain carbon austenite has been studied by many investi-gators.'-3 It was shown that cobalt displaces the TTT curves to shorter times and diminishes the harden-ability. The interpretations given for this effect of cobalt are conflicting. According to E. Houdremont,4 cobalt increases the transformation rate of austenite because it increases the diffusion of carbon as shown in the experiments of E. Houdremont and H.Schrader,' R.Smoluchowski,5 and M. Blanter.6 On the other hand, M. Hawites and R. Mehl3 deny on the basis of their own experiments any effect of cobalt on the diffusion of carbon and they assume that an explanation should be found in an eventual effect of cobalt on the mechanism of nucleation and growth of pearlite. W. C. Hagel, G. M. Pound, and R. F. Mehl7 have shown by calorimetric measurements that cobalt increases the free energy of the austenite-pearlite transformation in an eutectoid steel and this result explains qualitatively the observed effect of cobalt on the rate of nucleation and growth of pearlite. The purpose of this research was to see by determination of TTT curves, if this same effect exists in 13 pct Cr steels. EXPERIMENTAL PROCEDURES The preparation of the alloys was carried out in an

Jan 1, 1960

By S. F. Ramseyer, E. A. Steigerwald

INFILTRATED structures represent composite materials which are capable of combining high-temperature strength with adequate low-temperature toughness and thermal shock resistance. Although copper- and silver-infiltrated tungsten structures are actually being used in rocket nozzle hardware, adequate understanding of the fracture mechanics of these composite systems is not available. Specifically the relative importance of the strength, ductility, and modulus of the infiltrant in determining composite properties is not known to the extent that optimum composites can be selected. The major portion of experimental effort in the area of composite strength has been devoted to fiber-reinforced systems1 or to systems where a discontinuous phase is imbedded in a relatively ductile matrix.2'3 In the case of high-temperature systems, which are composed of a relatively brittle matrix, such as tungsten or an oxide, a continuous phase exists for the propagation of a crack. The method by which the presence of a conjugate ductile continuous phase influences the gross properties of the composite represents an area which requires further investigation. This technical note presents results which evaluate the effect of infiltrant strength on the strength of the tungsten-base composite. A tungsten matrix and copper-base infiltrant were selected for the initial studies because of the ease of fabrication. Tungsten structures with nominally 20 and 30 pct porosity were evaluated. The porosity was controlled by varying the initial powder size and a ratio of open-to-total porosity greater than 95 pct was obtained by selective sintering cycles. The processing sequence involved hydrostatic pressing followed by a 72-hr presinter in hydrogen at 2000° F and a final sinter at 4000°F for 4 hr in vacuum. The 20 pct porous structure was obtained

Jan 1, 1965

By Noel Jarrett, Allen S. Russell, Bernard M. Starner, Stanley C. Jacobs

A process has been developed to refine high-grade commercial aluminum to 99.99 pct purity. This enzploys precipitating titanium, vanadium, and zirconiu~ as borides. The upgraded liquid is partially crystallized under conditions that prevent massive freezing. The resulting crystals are compacted and washed free of adhernig impure liquid aluminum by melting the top crystals while draining off the liquid. Finally, the bottorn portion of the crystal bed is melted and removed as the pure product. Leakage from the crystallizat~on vessel is prevented by a layer of alumina granules that are not wetted by the aluminum. ALUMINUM of 99.99 pct purity is desired in a variety of applications. These include electrolytic capacitors, catalyst carriers, decorative trim for automobiles, aluminum powder, and high-strength alloys. This market was for many years filled by refining commercial-purity aluminum in a three-liquid-layer electrolytic cell of the type originally proposed by Hoopes. To meet the expanding need for lower-cost high-purity aluminum, a refining process based on chemical precipitation and fractional crystallization was developed. The availability of this super-purity metal was announced in November 1961, and three patents1-3 relating to the process were issued in 1965. An alternate process, comprising continuous fractional crystallization of a portion of a liquid-aluminum feed stream under conditions of strong agitation at the surface of the growing crystals, was published by Dewey4 in 1965. Earlier proposals by Larsen 5 and by Regner6 also emphasized the advantage of rapid agitation of the melt in the region of the crystallization zone. johnson 7 more recently proposed extracting purified aluminum from an alloy by mixing crystals of pure aluminum into the molten alloy, allowing them to grow, and removing the pure aluminum as by casting. Aamot's 8 recent patent describes a freeze refining process that involves controlled partial freezing against cooled moving retort walls. The Alcoa process to produce high-purity aluminum is schematically described in Fig. 1. Relatively pure aluminum is treated with boron in a furnace (a) to precipitate high melting point impurities, the supernatant liquid is transferred to a crystallization vessel (b), the liquid is partially crystallized with mechanized "tamping" (c), the remaining impure liquid is tapped out and the crystal bed partially and directionally re-melted to wash the underlying crystals (d), and the balance of the crystals is melted and withdrawn as high-purity aluminum (e). PRINCIPLES OF FRACTIONAL CRYSTALLIZATION Commonly encountered impurity elements form two types of systems with aluminum. Titanium, vanadium, and some other transition elements in periodic groups IV, V, and VI are the high melting point impurities. Initial solidification of aluminum containing small percentages of these elements will produce solid markedly enriched in them at temperatures slightly above the freezing point of high-purity aluminum. Most other elements, such as silicon and iron, produce eutectic type reactions with aluminum. In this case the first solid formed on initial solidification at temperatures slightly below the freezing point for high-purity aluminum is markedly depleted while the remaining liquid is enriched in these elements. The equilibrium change in composition during solidification of aluminum contaminated with silicon, iron, or titanium is illustrated in Fig. 2. Here, for clarity, the temperature scale is expanded beyond the

Jan 1, 1968

By C. W. Spencer, B. F. Addis, G. H. Bishop, C. A. Steidel

STUDIES of the inter granular attack of metals by liquids have generally been confined to polycrys-talline specimens. This note reports the results of preliminary studies of the penetration of bismuth-rich Ni-Bi liquids into oriented bicrystal specimens of nickel. It is found that isothermal penetration follows a parabolic rate law and shows a definite anisatropy with respect to direction on the grain boundary surface. Nickel bicrystals containing < 100> tilt boundaries were grown using the Czochralski method. Relative misorientation of the parent crystals was controlled to ± 1deg. The boundaries are straight in the growth direction, i.e., the common <100>, and generally straight in the transverse direction, as shown in Fig. 1. The starting material, Inco HPM grade nickel was contained in a recrystallized alumina crucible and maintained under argon. Bicrystals typically contain 30 ppm C, less than 10 ppm S, O, N, and 50 ppm residual metallics, principally iron and silicon. Specimens, as schematically illustrated in Fig. l(c),were cut from bicrystal ingots using a thin water-cooled abrasive wheel. To insure removal of all residual strain, which accelerates the penetration, specimens were round through 600 grit silicon-carbide, chemically polished, and annealed for 4 hr at 1375°C under argon. The procedure described by Cheney et al.1 for exposing specimens to

Jan 1, 1962

By I. Stapf

Systematic investigations on silver-rare earth metal systems have been extended on the Ag-Ce system in order to clarify the discrepancies reported in literature. The phase diagram has been reinvestigated on the base of thermal analyses and of microstructure examination on cast and annealed specimen. All intermetallic phases Ag4Ce, Ag3Ce, Ag2Ce and AgCe show no extended range of homogeneity, they melt congruently fm), or decompose peritectically (d) at 815 °C (d), 1030 °C (m), 855 °C (d) and 855 °C (m), respectively. The system shows eutectics at 793 °C/10 at.%, 780 °C/42 at.%, and about 505 °C/81 at.% Ce. d-Ce dissolves up to 2 at .% Ag and decomposes metatectically at 710 °C. Furthermore, the phase transformation of the intermetallics would be clarified. The phases Ag5Ce and Ag51Ce14 reported in literature could not be verified.

Jan 1, 1984

By James F. Lewis

THE hematite iron ore mines east of the Hudson River are confined to a strip of country ten to fifteen miles wide, commencing on the south, near Fishkill, running northeast through Dutchess County, and striking the southeast corner of Columbia County, extending into Litchfield County, Conn., known there as the Salisbury mines, cropping out again at and near West Stockbridge, Lanesboro, and Cheshire, Mass., also in Bennington County, Vermont. The ores are found in beds or deposits and in veins, with a limestone ledge on one side and slate on the other, from six to thirty feet from the surface. Portions of it are quite solid, called rock ore, but

Jan 1, 1877

Pulverized Fuel Combustion The apparatus shown in the illustration is a complete equipment f r supplying coal to boiler and metallurgical furnaces, cement and lime kilns, dryers, and to all furnaces requiring a temperature and quality of fame under prompt and easy control. It is claimed that the Aero Pulverizer makes practicable the highest efficiency obtainable from burning coal. It makes coal burn like a gas, a flame, the physical and chemical character of which is regulable- a flame that may be elongated or shortened, thus placing the zone of highest temperature where needed- a flame that may be made oxidizing, reducing, or neutral, as occasion may require. The coal is burned as pulverized, and there is no storage of the powder with its attendant hazard. Artificial drying before pulverizing is not necessary if the coal supply be sheltered from rain and snow. Where the Aero is used, it is wholly a furnace question whether a dryer should be installed; it is not at all a pulverizing or storage question. Labor is reduced to a minimum. Slack coal at low cost yields its last B.T.U.

Jan 11, 1915

By Paul T. Allsman

Passage of the Mining Act of 1866, superseded by the Act of 1872, was the first major entry of the Federal Government into the problems of mining. Such a law was necessary simply to help re- solve a number of disputes in mining. Now, however, a hundred years later, the extent of government involvement in the mineral industry often comes as a shock to the mining engineer who has reached management level. In fact, he has been poorly prepared for an understanding of the role of government in the industry and he becomes frustrated, even hostile. In our political system, private industry is responsible for producing minerals and the Government sees to it that production will be adequate for a peace-time economy and for any emergency. There have been great social and political changes since World War I1 with the result that the Government&apos;s participation in our society has steadily increased. A new dimension in business and government relations has been introduced which should be examined more closely.

Jan 5, 1966

By Conrad E. Hesse

To increase the durability of paint exposed to the weather, it is necessary to protect the oil with a substance that is itself unaffected by the elements. The so-called " metallic " paints, containing ochre,

Jan 1, 1891

By R. W. Leonard

A method of accurately determining the value of gold-bearing ores and gravels with a compact field-outfit is much desired by prospectors, especially when the work lies in a district far removed from railways or good wagon-roads. We are all familiar with the fire-assay of gold-ores, and fully recognize its accuracy and value; but only those who have tried to determine the value of a gold-bearing vein as a commercial venture, from fire-assays of selected samples, know how misleading is the information thus obtained, however carefully and honestly the samples may be selected. The reasons are that, for the fire-assay a very small portion of ore is treated (rarely more than six assay-tons, or a little over one-third of a pound), and a minute particle of the precious

Jan 1, 1896

By E. P. Klier

THE work of Klier and Lyman1 on the bainite reaction has led to the full description of this reaction for medium-carbon low-alloy steels. Certain experimental data reported by Klier and Lyman appear, however, to be improbable of obtaining in very high-carbon steels. The study herein reported consists of an analysis of the transformation characteristics of a 3 per cent chromium, 1 per cent carbon steel by means of X-ray and metallographic methods. From the results obtained it is concluded that the bainite reaction in this steel is more complicated than that reported by Klier and Lyman for the low-carbon low-alloy steels. However, the mechanism of bainite formation in this steel appears to be essentially the same as proposed for the low-carbon low-alloy steels with the modification that the first volumes to transform are carbon-rich rather than carbon-poor. EXPERIMENTAL PROCEDURE The analysis of the steel studied was: Cr, 2.89; C, 1.02; Mn, 0.33; Si, 0.35; S, 0.012; P, 0.020. The stock was received from the Carpenter Steel Co. in rolled bars. Specimen Preparation Specimens were austenitized at 1200°C. (2192°F.) for 25 min. in purified nitrogen. The resultant A.S.T.M. austenite grain size was 0-1. Isothermal transformation was allowed by quenching the specimens into liquid metal baths controlled to ±5°C. at 540°C. (1004°°F.) and above, and to ±2°C. at 490°C. (914°°F.) and below. Following the desired degree of transformation all specimens were water quenched. Metallographic Examination Specimens 1/4 in. round by 1/4 in. were used for metallographic examination. Etchants used were Vilella&apos;s reagent (1 gram picric acid, 10 ml. hydrochloric acid to make l00 ml. ethyl alcohol solution) and alkaline sodium picrate (electrolytic). Vilella&apos;s reagent was effective in revealing all microconstituents, while the alkaline sodium picrate developed the carbon-rich structures or carbides only. X-ray Examination Two X-ray techniques were used-the Debye-Scherrer method and a back-reflection method. The small specimens necessary for the Debye-Scherrer method were austenitized and then allowed to transform, or were cut from the larger metallographic specimens. The metallographic specimens were used for the back-reflection X-ray analysis. When it was desirable to determine the structure of the carbide present, sliver specimens were electrolytically etched to develop a carbide coating, then were exposed in the cameras. This technique was frequently necessary to allow positive identification of the carbide.

Jan 1, 1945

By J. B. Newkirk, A. H. Geisler

Certain of the permanent magnet alloys provide ideal systems for the study of the kinetics of the precipitation reaction and the correlation of structure with properties. One such system, Cu-Ni-Fe, was found by Bradley1,2 to exhibit a coherent transition state in the precipitation process analogous to that reported for Al-Cu alloys somewhat earlier.3 The attractiveness of some perrnanent magnet alloys for study lies in the fact that vertical sections of the ternary phase diagram in certain regions of composition (Fig I) have as their prototype the binary Ni-Au diagram. Alloys of this type decompose into products that have the same crystal lattice type but only slightly different lattice parameters. The advantages that such alloy systems oA&apos;er for study over the usual in which an intermetallic compound is formed are many: 1. Since the precipitate has the same crystal strutture as the matrix, complex atomic movements are not required to form the new lattice. 2. Similarly, complex orientation relationships are not involved for both the matrix and the precipitate would be ex. petted to have the same orientation. 3, Small &,registry of the decomposition products at equilibrium (in contrast with Cu-Ag alloys) is conducive to extensive coherent growth in the transient state and thus the transition lattice can be detected by the usual X ray diffraction methods. 4. Finally, the relative quantities of precipitate and depleted matrix can be varied from 0 to 100 pet* thus permitting wide freedom for the study of the effect of cornposition on coherent growth and properties. In the Cu-Ni-Fe alloys of appropriate composition, the face-centered cubic precipitate and also the depleted matrix when first formed are coherent with the parent matrix.1&apos;2 The two have the same <Jo parameter as the original matrix but they are both tetragonal; the precipitate has an axial ratio c/a < I while that of the depleted matrix is c/a > I. When coherency is lost they assume the normal face-centered cubic structure with the depleted matrix having a lattice parameter greater than the original matrix and that of the precipitate less. Such a mechanism would also be expected for CU-Ni-CO alloys because of the similarity in constitution but this had not been demonstrated. The Present investigation was conducted on a CU-Ni-CO alloy. The constitution diagram and magnetic properties of these alloys have been fairly well established, however, no previous determinations of mechanism of precipitation and no correlation of structure with properties had been made. Thus, an alloy of this system Was chosen for a comprehensive investiga-

Jan 1, 1949

By J. Redstone, A. R. Laplante

Sidbec-Normines operates six large iron ore concentrate regrinding mills in parallel and open circuit at its Port-Cartier pelletizing plant. Grinding kinetics in these mills were characterized for slurry densities varying between 70 and 89% solids, using a lumped parameter size discrete model. Optimum grinding conditions were encountered at 83.5 to 84% solids. Higher densities decreased the normalized selection function and increased slurry short-circuiting, yielding a sharply coarser mill discharge. At lower slurry densities, the normalized selection function decreased and the mill discharge coarsened slightly. The grinding kinetic model predicted particle size distributions within the mill. These were found to vary significantly from the feed to the discharge end. This is likely to cause nonlinear breakage kinetics.

Jan 1, 1985

By D. W. Philips

The problem of strata control has of necessity been prominent in mining, and accounts of individual experience and research abound in the literature of most mining countries. Organized rescarch began in Britain by the formation of a committee, upon the recommendation of the Safety in Mines Research Board in 1923, to investigate methods of reducing accidents from falls of roof in coal mines. This committee examined current practice in supporting underground workings in the principal coal fields, and its findings have been published in the Board&apos;s publications.&apos; - Toward the end of these investigations it was suggested by the Chief Inspector of Mines that committees of the several mining institutes be formed to examine the problem in their respective districts. The formation of these committees marked a new phase in research on strata control. The work, though being done in the separate coal fields, followed a scheme outlined by the chief Mining Engineer of the Research Board, and was coordinated by his office. FACTORS INVOLVED The subject is being considered in Britain from two aspects: 1. To provide. by supports, means to prevent falls of fractured ground. 2. TO develop methods whereby the strata can be maintained in the least broken condition and thus make falls less likely. The first aspect is the one that will most likely lead to immediate results from the accident standpoint. It depends largely upon the assimilation of already acquired knowledge regarding the properties of supports and their correct application. The second aspect is perhaps more fundamental, and involves also the properties of the strata and their behavior under the influence of the forces induced by mining. The problem involves many natural factors that cannot be controlled, such as depth, inclination and thickness of seam and nature of the rocks. Other factors, which may be considered to a certain extent controllable, cannot be varied readily and with sufficient frequency to facilitate easy investigation; some of these are: rate of advance of the working face, length of face, direction of the face with regard to cleat and inclination, system and arrangements of rock packing behind longwall faces. In any given case the very many factors present have a mutual influence upon the effects produced in the mine. For example, a study of the effects of rate of advance cannot be done without considering the effects of other factors such as nature of strata, direction of face and quality and arrangement of supports. Conversely, the length and direction of a working face

Jan 1, 1947

By D. W. Philips

The problem of strata control has of necessity been prominent in mining, and accounts of individual experience and research abound in the literature of most mining countries. Organized rescarch began in Britain by the formation of a committee, upon the recommendation of the Safety in Mines Research Board in 1923, to investigate methods of reducing accidents from falls of roof in coal mines. This committee examined current practice in supporting underground workings in the principal coal fields, and its findings have been published in the Board&apos;s publications.&apos; - Toward the end of these investigations it was suggested by the Chief Inspector of Mines that committees of the several mining institutes be formed to examine the problem in their respective districts. The formation of these committees marked a new phase in research on strata control. The work, though being done in the separate coal fields, followed a scheme outlined by the chief Mining Engineer of the Research Board, and was coordinated by his office. FACTORS INVOLVED The subject is being considered in Britain from two aspects: 1. To provide. by supports, means to prevent falls of fractured ground. 2. TO develop methods whereby the strata can be maintained in the least broken condition and thus make falls less likely. The first aspect is the one that will most likely lead to immediate results from the accident standpoint. It depends largely upon the assimilation of already acquired knowledge regarding the properties of supports and their correct application. The second aspect is perhaps more fundamental, and involves also the properties of the strata and their behavior under the influence of the forces induced by mining. The problem involves many natural factors that cannot be controlled, such as depth, inclination and thickness of seam and nature of the rocks. Other factors, which may be considered to a certain extent controllable, cannot be varied readily and with sufficient frequency to facilitate easy investigation; some of these are: rate of advance of the working face, length of face, direction of the face with regard to cleat and inclination, system and arrangements of rock packing behind longwall faces. In any given case the very many factors present have a mutual influence upon the effects produced in the mine. For example, a study of the effects of rate of advance cannot be done without considering the effects of other factors such as nature of strata, direction of face and quality and arrangement of supports. Conversely, the length and direction of a working face

Jan 1, 1947

By R. K. Ham, M. L. Wayman

TD-Nickel has been broken in tension and in fatigue at voom temperature. Rod specimens failed in tension by necking, with axial cracks attributed to voids elongated in the extrusion direction. Fatigue specimens failed in shear. Thin-film electron microscopy showed that the subgrain structure of TD-Nickel was very stable, and that particle-matrix detachment was very difficult, in tension and fatigue. TD-Nickel softened slightly during fatigue but had a high fatigue ratio (0.5at 10&apos; cycles). Fractography suggested that Stage I fatigue crack propagation is greatly extended in TD-Nickel. Td-NICKEL* is a dispersion of 2 pct by volume of thoria (ThO2) in nickel, produced by powder-metallurgical methods including compaction, sintering, and extrusion. The spherical thoria particles, which may have a mean diameter of a few hundred angstroms, are dispersed with a mean planar spacing of a few thousand angstroms. By a combination of cold working and annealing, a subgrain or cell structure of dislocations intimately associated with the dispersion can be produced.&apos; This gives the material useful tensile properties which are extremely resistant to exposure to high temperatures.&apos;-= At the same time, the material shows considerable ductility.3&apos;4 At the beginning of the present work, it was considered of great interest to investigate the mechanical stability of TD-Nickel under conditions of fatigue. On the one hand, materials which derive strength from a cold-worked structure are unstable in that they are susceptible to fatigue softening: in addition, the presence of discontinuities such as the particle-matrix interfaces might be expected to assist in the initiation and propagation of fatigue cracks, in that they may provide local concentrations of internal stress and sites for the initiation of voids." On the other hand, the substantial ductility of TD-Nickel suggests that if it obeys Coffin&apos;s relation8 (or the more refined form proposed by Manson9) it should have good fatigue resistance. The initial purpose of this investigation was to assess the importance of these factors. Also, relatively little fundamental work has been done on the mechanism of fatigue in dispersion-strengthened materials. Work on overaged A1-4 pct CU10-12 revealed a very large Bauschinger effect indicative of internal stresses at the particles, and very great fatigue hardening1&apos; presumably due to the multiple slip stimulated by these internal stresses, followed by softening which was initially due to softening in the matrix, but later might have arisen from cracking at the particle-matrix interfaces. The study of overaged Al-4 pct Cu could not settle this latter point by the electron microscopy of thin films, since the dispersion is too coarse. A previous study of the fatigue of internally oxidized copper13 was complicated by inter granular failure, attributed to oxide particles at grain bouhdaries; internal oxidation of single crystals, however, improved their fatigue properties.&apos;3 Investigations of SAP (sintered aluminum powder) are complicated by the complex particle shapes, and the possibility of continuous internal oxide films.14 It was hoped to avoid these difficulties with TD-Nickel, which had the further advantages that it was commercially available and suitable for study by the thin-film technique. 1) MATERIALS AND EXPERIMENTAL PROCEDURE TD-Nickel was purchased from the Driver-Harris Co. as 3/9-in.-diam rod which had been extruded, swaged, and "stress-relieved" (normally at 1010°C for 1 hr). Continuous-radius fatigue specimens with a minimum diameter of -0.1 in. were ground to shape and electropolished in 40 pct phosphoric, 35 pct sul-furic, 25 pct water at 25oC, with a stainless-steel cathode, at -6 v. Fatigue tests were carried out at room temperature with a Sonntag SF-1-U machine operating in push-pull at 1800 cycles per min, and in an Instron TT-C-L modified for reversed stressing at 26 cycles per min as described elsewhere.10 Round tensile specimens were ground with 0.85-in. gage lengths of 0.135 in, diam, electropolished, and tested in a Tinius Olsen hydraulic machine. The surfaces of fatigue specimens were examined with a Reichert metallograph. Discs for electron microscopy with a Siemens Elmiskop I were spark-cut 0.01 in. thick with a modified Servomet 11 employing a tool of moving molybdenum wire, cleaned in 50 pct acetic, 30 pct nitric, 10 pct phosphoric, and 10pctsul-furic at 85oC, and thinned by the window method in the electropolishing solution at -20°C and -6 v. Two-stage replicas (parlodion, then Pt-50 pct C self-shadowed at 40 deg) were taken from fatigue fracture surfaces for electron microscopy. Plane sections parallel to the specimen axis and containing the direction of fatigue crack propagation were polished, etched with Carapella&apos;s reagent, and examined optically. Transmission Laue X-ray photographs of as-received material electropolished to a point were used to determine preferred orientation. 2) RESULTS 2.1) The Structure of As-Received Material. Grains -1 µ diam and elongated 20 to 30 u in the direction of the rod axis were observed, With&apos; elongated "intergran-ular" voids (-4 p diam and -90 µ long and identified as such using longitudinal and transverse sections and

Jan 1, 1968

By AIME AIME

COUNCIL PRESIDENT OF THE COUNCIL. CHARLES KIRCHHOFF NEW YORK, N. Y. (Term expires February, 1912.) VICE-PRESIDENTS OF THE COUNCIL. BENJAMIN B. LAWRENCE NEW YORK, N. Y. JOSEPH W. RICHARDS SOUTH BETHLEHEM, PA. ALBERT SAUVEUR CAMBRIDGE, MASS. (Term expires February, 1912.) S. B. CHRISTY BERKELEY, CAL. W. A. LATHROP PHILADELPHIA, PA. GARDNER F. WILLIAMS WASHINGTON, D. C. (Term expires February, 1913.)

Oct 1, 1911

By J. W. Powell, F. H. Spedding

A complete review of the use of chelating agents in the sepa ration of rare earths by ion-exchange is given as well as a concise description of the recent pilot-plant operations of the Ames Laboratory. The two chelating agents which show the greatest promise are ethylenediamine-N,N,N&apos;,N&apos;-tetraacetic acid and N&apos;-(2-hydroxyethyl)ethylenediarnine-N,N,N &apos;-triacetic acid. The first successful separations of rare earths by ion exchange were reported in a collection of papers which appeared in the November, 1947, issue of the Journal of the American Chemical Society.1&apos;9 Some of this work was performed at the Ames Laboratory of the A.E.C., the remainder at the Oak Ridge National Laboratory. The processes developed at Oak Ridge, as well as some of the early Arnes methods, employed 5 pct citric acid-ammonium citrate eluant at low pH and were carried out on either H+-state or NH:-state resin beds. These techniques were successful for the separation of small quantities of either naturally occurring or radioactive rare earths and are still used for the isolation of rare-earth activities from fission products. Concentrated citrate is not economical, however, for use in moderate or large-scale rare-earth separations. For this reason, the Ames Laboratory turned its attention to lower concentrations and higher pH&apos;s in order to make more effective use of the eluting agent.10-14 Although elutions have been performed successfully over a wide range of conditions, 0.1 pct citrate at a pH of 8.0 is highly recommended for use on H+-state resin beds.15,16 Elu-tion with 0.1 pct citrate in the pH range from 5 to 9 brings about the separation of the constituent rare earths into a series of flat-topped elution bands which progress down the resin bed, head to tail, without actually pulling apart as do the rare-earth peaks which develop when trace quantities are eluted with 0.25M (5 pct) citrate at low pH&apos;s. Because of this, elution with 0.1 pct citrate at pH 8.0 do not produce pure rare earths unless sufficient quantities are present to provide developed bands which are at least several inches long on the columns. Although other eluting agents have proved more effective than citrate solutions, articles concerning the use of citric acid for separating rare earths still appear in the literature occasionally. For example, Ketelle and Boyd17 reported some further studies on the separation of rare earths with 5 pct citrate in 1951. They used 270 to 325 mesh Dowex-50 columns at 100°C and a pH of 3.28. vickery18 compared the effectiveness of a number of eluants for the separation of rare earths on NH+4 state Dowex-50 in 1952. He found that citric acid was more efficient than acetic, malic, tartaric, and aminoacetic acids. In 1953, Mayer and Freiling18 reported that citrate was inferior to malate, glycolate, lactate, and EDTA for the resolution of Sm-Eu and Y-Tb mixtures on 250 to 500 mesh, NH+4-state, Dowex-50 at 87°C. pinta20 used 5 pct citrate in the pH range 2.8 to 3.4 to obtain some rare earths for analytical work the same year. Trombe and Loriers21 reported the use of citric acid in their laboratory to separate rare earths in kilogram quantities. Lariers and Quesney22 reported some separations with citrate in 1954. They used 5 pct citrate at pH 2.8 to separate yttrium and the yttrium-group rare earths from the cerium-group rare earths. briers23 used 5 pct citrate at pH 3.2 and 90°C as late as 1956 to isolate thulium in fair purity. For the separation of tracer quantities of rare earths, Mayer and Freiling19 have recommended pH 5.00, 0.24M lactate at 87 °C on 250 to 500 mesh, NH+4-form Dowex-50. Freiling and Bunney24 have also employed lactic acid for the separation of fission-product rare earths. Cunninghame, Size-land, Willis, Eakins, and Mercer25 have reported a 4-hr separation of Y, Eu, Sm, Pm, Nd, and Pr with 1M lactic acid at pH 3.25 on Zeokarb-225 at 87°C. Stewart, et al.,26 reported separation factors for rare earths distributing between Dowex-50 and 0.25M glycolic acid. stewart27 also reported a 30-61 separation of Y, Tm, Er, Tb, and Lu tracers with buffered, 0.25M glycolic acid containing 0.05 pct Aerosol OT. The resin bed was 400-mesh Dowex-50 (X12). The pH of the ammonia-buffered eluant was 3.5. Various aminopolyacetic acids have also been used to obtain varying degrees of separation of the rare earths. In 1951, Fitch and Russell28 investigated iminodiacetic acid (IDA) and nitrilotriacetic

Jan 1, 1960

By R. L. Skaggs, D. T. Peterson

The effect of carbon in solid solution on the plastic behavior of thorium was studied by measuring the flow stress of Th-C alloys from 4.2" to 573°K and at several strain rates. Carbon was found to strengthen thorium primarily by increasing the thermally activated component of the flow stress. The strengthening due to carbon was directly proportional to the carbon content and decreased rapidly with increasing temperature up to 423" K. The flow stress also increased with increasing strain rate. The strengthening appears to be due to a strong short-range interaction between carbon atoms and dislocations. A yield point was observed in the Th-C alloys which increased with increasing carbon content. JTREVIOUS study of the mechanical properties of thorium has been confined largely to the measurement of the engineering properties. Work prior to 1956 has been summarized by Milko et al.1 who reported that additions of carbon to thorium sharply increased the room-temperature strength. In addition, the yield strength was observed to decrease rapidly over the temperature range from 25" to 500°C. In 1960, Klieven-eit2 measured the flow stress of thorium containing 400 ppm C. He found that over the temperature range from 78" to 470°K the flow stress was strongly dependent on temperature and rate of deformation. A drop in the load-elongation curve, or a yield point, was observed over most of the above temperature range. Above 470°K, the flow stress was nearly independent of temperature and strain rate. This strong temperature and strain rate dependence of flow stress is not generally observed in fcc metals. It is, in fact, more typical of the behavior reported for bcc metals. Bechtold,3 Wessel,4 and conrad5 have pointed out the striking difference between the commonly studied bcc metals and fcc metals in regard to the effect of temperature and strain rate on the flow stress. Zerwekh and scott6 studied the plastic deformation of thorium reported to contain 12 ppm C. They found that this material did not obey the Cottrell-Stokes law as expected for fcc metals. In addition, they found values of the activation volume smaller by an order of magnitude than expected for an fcc metal. They concluded that thorium was strengthened by a randomly dispersed solute. Thorium differs from many other fcc metals that have been studied extensively in that it shows a relatively high carbon solubility at room temperature. Mickleson and peterson7 report the solubility limit at room temperature to be 3500 ppm C. The lowest value reported is that of Smith and Honeycombe8 who report the limit to be 2000 ppm C at 350°C. The pres- ent investigation was a systematic study of the flow stress and yield point phenomenon of thorium over a broad range of carbon content, temperature, and strain rate. EXPERIMENTAL PROCEDURE The thorium used in this investigation was produced by the reduction of thorium tetrachloride with magnesium as described by Peterson et a1.&apos; Chemical analysis of the original ingot after arc melting and electron beam melting is shown in Table I. Alloys were prepared by arc melting this thorium with high-purity spectrographic graphite. Threaded specimens with a gage length 0.252 in. diam by 1.6 in. long were used for the constant stress or creep measurements. These specimens were machined from rod which had been cold-rolled and swaged to % in. diam. Tensile specimens were prepared by swaging annealed 3/8 -in.-diam rod to 0.102 *0.001 in. The as-swaged wire was cut to lengths of 2 in., annealed, and the center 1-in. gage length elec-tropolished to 0.100 ±0.001 in. The specimens were gripped for a length of 3 in. at each end by a serrated four-jaw collet which was tightened by a tapered compression nut. No slipping occurred in the grips and negligible deformation was observed outside the 1-in. gage length. Both the creep and tensile specimens were annealed at 730°C under a vacuum of 1 x X Torr. The resulting structures consisted of equiaxed recrystallized grains with a grain size of 3200 grains per sq mm for the tensile specimens and 2200 grains per sq mm for the creep specimens. After the specimens were prepared, samples were analyzed for nitrogen, oxygen, and hydrogen. The results of these analyses are given in Table 11.

Jan 1, 1969

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Jan 4, 1978