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By R. W. Kewish

The preparation of massive uranium metal containing very low concentrations of a number of light elements by bomb reduction of UF4, with calcium is described. Details of procedures are given for preparing high-purity ingredients for the bomb reduction. The as-reduced uranium metal contained, on the average, less than the following amounts of light element impurities, in ppm: Li, 0.1; Be, 0.1; B, 0.1; C, 25; 0, 70; Na, 1; Mg, 3; Al, 2; and Si, 7. Other impurities for which the metal was examined averaged, in ppm: Ca, < 10; V, < 10; Cr, 2; Mn, 6; Fe, 50; Co, < 5; Ni, 8; and Cu, 1. THE preparation of very high-purity uranium metal in massive form for research purposes is of great importance. Recently the kilogram-scale preparation of uranium metal containing less than 70 ppm of detected impurities was accomplished by Blumen-thal and coworkers by vacuum remelting of high-purity crystals of uranium obtained by fused salt electrolysis.1"3 Albert and coworkers4 have reported successful experiments in lowering the concentrations of certain impurity elements in uranium, notably iron, to a few ppm by the zone-melting method. The present paper describes the preparation of high-purity massive uranium metal by the bomb reduction of UF4, with calcium. Early in 1951 a program was undertaken at the Los Alamos Scientific Laboratory to prepare uranium metal of very high purity with respect to a number of the light elements. The methods considered for this purpose were 1) bomb reduction of a uranium halide with calcium, 2) electrolysis of fused salts, and 3) hot wire decomposition of UI4, The first of these processes had been used extensively at Los Alamos since 1943 (and still is used) for the production of uranium metal.5 In considering the three processes it was evident that either of the last two would require an extensive development program with no certainty of success. On the other hand, a study of available data showed that uranium metal of very high purity with respect to some light elements had occasionally been made in routine processing by the first method. It was therefore decided that an intensive study of the bomb-reduction process would be made to see if it could be improved to yield uranium metal with very low concentrations of light elements. DEVELOPMENT OF PROCEDURES The bomb-reduction process used at Los Alamos consists of reducing UF4 with calcium, using iodine as a booster. The reaction is carried out in a magnesium-oxide crucible enclosed in a steel bomb. Argon is used in the bomb to avoid objectionable side reactions which would occur in the presence of air. All ingredients for this bomb-reduction process were examined as possible sources of light elements. It was known that high-purity UF4 was required. The calcium used in the reductions was a source of carbon and magnesium. The magnesium-oxide crucibles were sources of boron, silicon, and magnesium. The iodine did not appear to be a source of any impurities. Pure UF4- The UF4 for bomb reduction is prepared from U3O3 , by successive reduction to UO2, with hydrogen and hydrofluorination of the UO2, with anhydrous HF. Since it was known that no impurities were normally introduced during the gas-solid reactions, effort was directed toward the preparation of high-purity U3O3. Of the many possible procedures for the purification of uranium solutions the following were investigated: 1) Precipitation of uranium peroxide. (Two procedures were tried. The first consisted of simultaneously adding hydrogen-peroxide and ammonium-hydroxide solutions to a uranyl-nitrate solution, containing citric and malonic acids, at such relative rates that precipitation was carried out at a constant pH of 1.5 The second consisted of simultaneously adding uranyl-nitrate, ammonium-hydroxide, and hydrogen-peroxide solutions to an aqueous solution

Jan 1, 1960

By E. C. Harder, E. W. Greig

Bauxite is known mainly as the ore from which aluminum is smelted but it has large use also in the manufacture of artificial abrasives and in the production of a number of useful chemicals as well as of aluminous cement "ciment fondu." An important and growing use is in the manufacture of refractory products. Composition Dana and earlier mineralogists gave the mineral formula of bauxite as A1203.21120 and the composition as A1202, 73.9 pct; H2O, 26.1 pct. A specific mineral of this composition has, however, never been identified by either microscopic, chemical or X ray examination, and therefore it is concluded that bauxite is a rock consisting of one or more aluminum minerals together with impurities. The term is now used synonymously with aluminum ore and it embraces gibbsite (hydrargillite or alpha trihydrate), A1203. 3H20 (A1203, 65.4 pct; H2O, 34.6 pct); boehmite (alpha monohydrate), A1203•H20 (A1202, 85 pct; H2O, 15 pct) ; diaspore (beta monohydrate), A1203•H20 (A1203, 85 pct; H2O, 15 pct), and mixtures in various proportions of any two of them. Bauxite of the Mediterranean region in Europe is predominantly boehmite, as in France and Istria, subordinately a mixture of gibbsite and boehmite, as in Dalmatia, or of boehmite (or gibbsite) and diaspore, as in Greece. The bauxite of North and South America, tropical Africa, Asia, and Australasia consists largely of gibbsite, but boehmite in appreciable amount occurs in many places. Corundum (A1202) is not included un¬der bauxite, although gradations from bauxite to emery or corundum exist. All bauxite, irrespective of the aluminum minerals composing it, contains certain impurities in variable amount, including silica in the form of clay minerals (kaolinite, halloy site, and others) or quartz, iron oxide (as hematite or goethite), titania (as leucoxene or rutile), iron sulfide (as pyrite or marcasite), iron carbonate (siderite), and calcium carbonate (as calcite); the last three mentioned in minor amount and of local occurrence only. Bauxite belongs to a group of partly consolidated materials called laterites, formed by surface weathering. This group includes also impure siliceous, ferruginous, and phosphatic bauxite and siliceous and aluminous iron ores and manganese ores and nickel and chrome laterites. Phosphorus and manganese minerals locally form important impurities in bauxite deposits. Properties Gibbsite is white or light shades of gray, cream or pink. Its hardness is 2.5 to 3.5; specific gravity, 2.3 to 2.4; crystal system, monoclinic, crystals tabular parallel to 001, often fibrous, concretionary, stalactitic; luster, vitreous to pearly; generally translucent; cleavage, parallel to 001; disassociation temperature, approximately 300°C. Boehmite, a relatively new and important mineral described by J. Boehm15 in 1925, confirmed and named by J. de Lapparen64 in 1930, has some properties not yet definitely determined. It occurs in grayish, brownish, and reddish shades. Its hardness is between that of gibbsite and diaspore; specific gravity, 3.01 to

Jan 1, 1960

By H. J. Booss

THERE is a considerable lack of data on thermody-namic properties of hard-metal alloys. Only two papers 1,2 give mean values of specific heat in an unknown temperature range; more recently the author3 gave more detailed information on the mean specific heat in the temperature range from 20" to -190° C.. EXPERIMENTAL 1) Method—Experimental procedure followed a method suggested by Oelsen and coworkers.4 It requires samples of some 100 g of weight. The time of measurement is prolonged (30 min) but one run allows the measurement of a lot of positions on the heat-content curve. Results4 were found to be in good agreement with "best values" given by kelley,5 Kubaschewsky and Evans,6 etal.

Jan 1, 1960

By J. E. Hilliard, J. W. Cahn

In this paper it is suggested that the degree of contiguity (or contact) between adjacent grains be described by three parameters which can be rigorously determined from measurements on a random plane of polish. An expression is also derived for the number of contacts per unit volume and it is shown that this quantity can-not, in general, be estintated from measurements on a random plane. IN a recent contribution1 Gurland has proposed various parameters for describing the degree of contiguity (or contact) between grains of the same phase in an alloy. To relate these parameters to measurements on a random two-dimensional section, it was necessary in most cases to make some assumption about the form of the structure. Since Gurland was specifically interested in sintered carbide structures, he chose, quite reasonably, to assume that the grains were constant-size spheres and that all the intersections were flat areas of constant radius. Since, as we will show, the relationships between the parameters and the measurements are strongly dependent on the grain shape and size distribution, it is evident that these assump tions will not be satisfactory approximations for a

Jan 1, 1960

By John B. Myers

Vermiculite is the commercial name used to describe a micaceous mineral that expands appreciably when heated. This process, called exfoliation, results in a light weight material. The light weight material is also called vermiculite, or more exactly, expanded vermiculite. Practically all uses of vermiculite are for the expanded material. Composition and Properties Vermiculite, in its natural state, has the characteristic micaceous habit and a perfect basal cleavage and readily splits into thin laminae, which are soft, pliable, and inelastic. The monoclinic crystal faces are often marked by triangular lines at 60° and 120°. The hardness varies from 1.5 to 2 or more, depending on the composition. The specific gravity varies from 2.2 to 2.7; specific heat 0.2; fusion temperature 2,000° to 2,500°F; luster pearly to greasy; color amber, bronze, brown, dark green, and black. Feel is like talc and sometimes soapy when wet. When heated quickly at elevated temperatures, vermiculite exfoliates by expanding at right angles to the cleavage into long wormlike pieces (the name vermiculite is from the Latin vermiculari, to breed worms). This important characteristic of expansion is believed to be a mechanical separation of the layers when the contained water is converted to steam. The increase in bulk volume of commercially prepared material is 8 to 12 times, but individual flakes may expand as much as 30 times. There is no expansion parallel to the cleavage. Vermiculite may also be expanded by several chemical processes such as soaking in hydrogen peroxide, weak acids and other electrolytes. The color changes during expansion. Heat-treated material changes to a light golden bronze or cream color depending on composition. The conditions of heating affect color. Heating in an oxidizing atmosphere produces reddish colors and heating in a reducing atmosphere produces dull gray colors. The iron is generally not oxidized during chemical expansion. Vermiculite is hydrated magnesium-aluminum silicate. Although there has been much research on the chemical and structural composition, there is not yet complete agreement on the exact formula and composition. This is to be expected since vermiculite is not a mineral of fixed composition and different workers have examined different varieties. It has been proposed that vermiculite is not a single species but a family of related minerals. This has also resulted in many names for the particular vermiculite found in a certain deposit. All of this difficulty arises from the very nature of its crystal chemistry. Unlike most minerals, certain crystal structure properties and the chemical composition can be changed by the ordinary forces of nature or in the laboratory. This would suggest that vermiculite be thought of more as a variable mineral rather than a group of related species. It was stated on page 261 of this volume in the chapter on Clay Minerals by H. H. Murray of the Georgia Clay Co., that vermiculite is an equidimensional, expandable clay mineral. Gruner (ref. 14, Chap. 12) showed that the structure consists of a layer made up of two silica tetrahedral sheets with a central magnesium, iron octahedral sheet separated by two layers of water molecules and adsorbed magnesium and calcium ions. Mathieson and Walker,2a in a recent publication, agree that vermiculite must be regarded as a true clay mineral. The characteristic properties of the mineral, such as high cation ex-

Jan 1, 1960

By P. K. Koh

Isothermal salt bath annealing of 0.014-in. thick 3 pct Si-Fe sheet was conducted at temperatures ranging from 927" to 1260°C in order to investigate the grain-growth behavior. Within the temperature range studied normal grain growth did not take place; instead nucleated grain growth prevailed. The nucleation frequency was found to increase with the annealing temperature, with corresponding decrease in grain diameter of ultimate secondaries after long-time annealing. Large secondaries grown by low-temperature isothermal annealing are essentially of (110)[001] orientation, and the (110)[001] texture is strong. The relatively small secondaries grown by high-temperature isothermal annealing also have orientations near (110)[001] as an average but widely scattered; thus the amount of (110)[001] texture is found to decxease with isothermal annealing temperature. Grain growth and texture development at various annealing temperatures can be described by families of sigmoidal curves with the time axis. ThE cube-on-edge (110)[001] texture and predominating large secondaries in fully annealed 3 pct Si-Fe are customarily produced by a 1100°C annealing of a primary recrystallized sheet. On annealing the primary recrystallized sheet above the temperature at which secondary recrystalliza-tion starts May and turnbull&apos; have demonstrated that secondary grains decrease in size as the temperature is increased. The phenomenon was attributed to a decrease in the (G/N) ratio where G is the growth rate of secondary grains and N is their nucleation frequency. In addition, the growth of grains in orientations rather far from (110) [0011 occurred. The present investigation is devoted to detailed rate studies of the same phenomenon. Mi-crostructure, magnetic anisotropy, and texture data were obtained on strips of 3 pct Si-Fe isothermally annealed for various lengths of time in a BaC12 salt bath at temperatures ranging from 927&apos; to 1260°C. The texture results are reported elsewhere.2 EXPERIMENTAL PROCEDURE Commercial 0.014-in. cold-rolled silicon-iron strip (3.16 pct Si), prepared by two stages of cold rolling with an intermediate short anneal, was given a decarburizing 3-min anneal at 800°C. Metallo- graphic studies indicated complete recrystallization. In order to provide a protective atmosphere and to obtain a rapid rise to an elevated temperature, a BaC12 and NaCl fused salt bath was used to heat samples isothermally at temperatures from 927" to 1260°C for various lengths of time. Torque magnetometer measurements were made on 1-in.-diam disc specimens before and after annealing, since magnetic torque curves supply information on textures and texture changes. Surface layers of the strip samples were polished and etched to reveal the grain structure. The diameters of grains were measured from micrographs at X100. The average value of diameters of matrix grains was established. Individual grains in the micrograph were cut out separately along grain boundaries. These grains were classified either as matrix grains or growth grains. The percent weight of growth grains in the cut-out patterns was reported as percent growth. Manv of the individual grains in the annealed samples were large enough to be X-rayed with a 5-mil beam for Lauegrams. Complete (110) pole figures were obtained for the primary recrystallized structure and short-time annealed structure with CoKa radiation at 30 kv in the back-reflection range, such as (220) for (110) poles, as described recently by Newkirk and ~ruce.~ Both the X-ray optics and the technique for pole figure differed slightly from those adapted previously.4

Jan 1, 1960

By A. J. Griest, A. P. Young, P. D. Frost

A study was made of the effect of ß grain size on the tensile ductility of a-ß titanium alloys haet treated to strengths in the range 165,000 to 180,000 psi. It was concluded that the primary cause of $ embrittlement is the large grain size which is obtained so rapidly in many a-ß titanium alloys when heated into the ß field. It was also found that grain-boundary a and acicular intragranular a in the microstructure are not necessarily detrimental to the tensile ductility if the prior ß grain size is sufficientlv fine. BETA embrittlement occurs in a-ß alloys when the finish hot-working or stages of the subsequent heat treatment have been done at temperatures in the ß field. In order to avoid this embrittlement, for-gings must be finished at temperatures under the ß transus. For better workability, it would be desirable to forge at temperatures in the ß field. For this reason, research has been conducted to determine the cause of ß embrittlement. Although ß grain size has been considered as a possible contributing factor to ß embrittlement, only limited research has been done to evaluate its effect. The effect of addition elements on ß grain growth in unalloyed titanium has been studied by Liu.&apos; Complete mechanical property data, however, were not obtained for correlation with grain size. Ogden and coworkers2 have investigated the effect of both a and ß grain size and grain shape in Ti-Cr-Mo alloys. Their data indicated that tensile ductility was relatively insensitive to ß grain size at annealed strength levels (140,000 psi ultimate). No study has apparently been made to determine the relationship between ß grain size and ß embrittlement in a-ß alloys heat treated to high strength (180,000 psi ultimate). The high-strength condition is that in which ß embrittlement is particularly severe. Beta grain size is not easily varied through the use of a range of annealing times and temperatures in the ß field, because of the rapidity with which ß grain growth occurs. Short-time heating techniques are needed to obtain the smallest ß grains. EXPERIMENTAL PROCEDURE In this research, the experimental procedure was as follows: 1) Tensile and microimpact specimen blanks were resistance heated to produce a range of ß grain sizes. 2) The tensile and microimpact blanks were then solution-treated in the a-ß field and aged to produce predetermined ultimate tensile strengths in the range 165,000 to 180,000 psi. Tensile and impact ductility were then correlated with a grain size for constant strength levels. Materials—The alloys Ti-6A1-4V, Ti-4A1-4Mn, and Ti-16V-2.5Al are representative of the heat-treatable a-ß types in which ß embrittlement can be severe. The compositions and ß transi of the heats studied are given in Table I. The Ti-16V-2.5Al heat was melted and fabricated to 1/4 in. round at Battelle; the other alloys were obtained as 1/4 in. round rolled from commercial heats. The micro-structures of the as-rolled alloys were fine a-ß mixtures. This structure is typical of titanium alloys hot-worked extensively in the a-ß field. Resistance-Heating Treatments to Establish ß Grain Size—For direit resistance heating, a 1/4-in.-diam s~ecimen was heated with a 3000-watt transformer rated for 1000 amp with adjustable secondary voltage. The apparatus included a spray quench fixture. Both heating and quenching periods could be automatically controlled. For temperature measurements, 28-gage Chromel-Alumel wires were tack-welded to the specimen at its midpoint. A high-speed recorder-controller was used to control the heating cycle.

Jan 1, 1960

By D. M. Baird

"THE Island of Newfoundland lies on the extreme eastern edge of the continent of North America and at the extreme northeastern end of the Appalachian geological province. Its belonging to the Appalachian province is shown in the geological history of the region and in the rock types and structures.Geosynclinal sedimentation in early and middle Palaeozoic times was interrupted by Taconic and, more profoundly, by Acadian, mountain building activity. Mid-Palaeo-zoic intrusions range from masses of serpentinized ultrabasic rocks to granite batholiths. A Carboniferous overlay of continental and shallow, drying sea types covers the earlier developed complex. Local basins in these times were filled with products of the erosion of tl1e earlier rocks, and, locally, grew the right kind of vegetation to make thin, discontinuons seams and pockets of coal. Post-early Pennsylvanian history is one of erosion and pene-planation with renewal of movement along many of the older fault systems."

Jan 1, 1960

By J. Chipman, T. Fuwa

The effects of various elements on the activity coefficient of carbon in liquid iron have been studied by two experimental methods: 1) equilibration with controlled mixtures of CO and CO2; 2) the solubility of graphite in the melt. Activity coefficient of C is increased by Al, Co, Cu, Ni, P, Si, S, and Srz. It is decreased by Cr, Cb, Mn, Mo, W, and V. THE thermodynamic properties of the iron-carbon binary system have now been fairly well established, although some uncertainty remains with respect to the exact location of some of the phase boundaries. The activity of carbon in ferrite and in austenite has been measured in the classic researches of R. P. smith&apos; while similar measurements by Richardson and ~ennis, and by Rist and chipman3 have established the values of the activity of carbon in liquid iron up to 1760°C. On the other hand, our knowledge of the effects of alloying elements on the activity of carbon in dilute solutions is restricted to Smith&apos;s experiments on systems Fe-C-Mn and Fe-C-Si in the austenitic range and to some more recent experiments of schwarzman4 in the a range. In addition there have been a number of determinations of the effects of various elements on the solubility of graphite in liquid iron, and from these the corresponding effect in saturated solution may be obtained. The purpose of the present study was to extend the investigation of the liquid system to include the effects of alloying elements upon the activity coefficient of carbon, principally in dilute solutions. Equilibrium measurements were made on the reaction C + co, = 2 CO (g) The prepared mixture of CO and CO,, diluted with argon, flowed over the surface of the liquid metal which, after several hours&apos; exposure to the gas, was quenched and anqlyzed. As in the earlier experiments, the principal experimental difficulty was in the deposition of carbon on the parts of the furnace at temperatures slightly below that of the metal bath. In order to minimize this difficulty, the ratio (Pco)2 /PCo2 was restricted to values not much higher than 100 atm, and correspondingly the carbon concentration in the metal seldom exceeded 0.30 pct. EXPERIMENTAL METHODS The method and apparatus were essentially the same as used by Rist and Chipman.3 The gaseous mixture consisting of highly purified CO, CO,, and argon, each controlled by a flowmeter, was led into the furnace and passed over the surface of the liquid-iron melt which was heated and stirred by high-frequency induction. One slight modification was made in that a molybdenum susceptor was placed outside the crucible for the sake of uniformity of temperature and to combat the tendency of carbon to precipitate on the crucible wall. Pure alumina crucibles approximately 25 mm ID were used. The charge consisting of about 30 g was made up of electrolytic iron, the alloying element to be added, and enough graphite to supply slightly more or less than the anticipated equilibrium carbon concentration. All metals used were of high purity. Metallic chromium, columbium, and vanadium were from special lots supplied by the Electro Metallurgical Co. Tin, copper, molybdenum, tungsten, cobalt, and nickel were of purest commercial grades. The electrolytic iron, after being cut to the proper size for charging, was prereduced by hydrogen at 850° to 1000°C to remove surface oxidation. The oxygen content of the reduced material was 0.002 pct. This treatment made it easy to control the carbon content of the initial melt. The charge was melted under the gas mixture to be used for the entire run. In some earlier melts the charge was melted under a stream of argon, but in this case some alumina was reduced from the crucible, and the aluminum thus absorbed in the melt was subsequently oxidized with the formation of a solid film of alumina on the surface of the melt. AS another safeguard against film formation, overheating of the bath was carefully avoided. All runs were made at a temperature of 1560°C. Under experimental conditions a charge of pure iron picked up 0.17 pct C in 3 hr and 0.23 pct C in 6 hr under an atmosphere for which the equilibrium concentration of carbon is 0.27. It is clear that the time required to reach equilibrium from an initially carbon-free melt would be very great. For this reason each experiment was started with a melt of known carbon concentration not far above or below the expected equilibrium value, and each melt was held at temperature for a period of at least 5 hr. Under such circumstances it was possible to chart the approach to equilibrium from both high-carbon and low-carbon materials. Temperature was controlled by frequent optical observation and adjustment and the metls were timed in such a way that the final 2 hr occurred during a time when electric power was steady; for example, 2 to 4 pm or after 11 pm. In melts containine volatile metals such as copper, tin, and mangane\e the time of holding was decreased somewhat in

Jan 1, 1960

By R. E. Ogilvie, A. R. Kaufmann, S. H. Gelles

The solid-solubility limits of iron in beryllium were determined between 850o and 1200oC by analysis of differential type multiphase diffusion couples, using an X-ray absorption technique. The maximum value of the solubility limit was found to be 0.92 ± 0.02 at. pct (5.46 wt pet) at the eutectic temperature 1225°C. The solubilities of nickel and beryllium were determined between 900°and 1200°C by the same technique and the maximum solubility was found to be 4.93 + 0.01 at. pct (25.2 wt pet) at the eutectoid temperature, 1065°C. A previously unreported high-temperature phase which decomposes eutectoidally at 1065 °C was found to exist in the beryllium-nickel system at a composition of approximately 8 at. pct Ni (36 wt pet) by diffision-couple analysis. The presence of this phase was confirmed by thermal analysis and metallo-graphic analysis of the structure resulting from the eutectoid decomposition. G. V. Raynor1 has treated the solid solubilities of some of the elements in beryllium on the basis of the "Hume-Rothery" rules2 which have been modified to include ionic size and ionic distortion effects. It was predicted that the solubility of iron and nickel in beryllium should be slightly less than that of copper. The lowering of the solubility, according to Raynor, is due to a more unfavorable relative valency effect and an ionic size effect. Kaufmann and corzine3 have compiled data on the solubilities of elements in beryllium and have discussed them in the light of the Raynor paper. These authors feel that, because the elements having the greatest solubility in beryllium systematically fall in the Group VIII and IB Columns of the periodic table, the electronic structure greatly influences the maximum solid solubility of elements in beryllium. The solubility of iron in beryllium was determined by Teitel and cohen4 as part of the study of the beryllium-iron phase diagram. The determination was carried out by X-ray and thermal analysis and according to the phase diagram presented, the maximum solubility of iron in beryllium is 0.41 at. pct (2.5 wt pct) at 1225oC. However, it is estimated that the uncertainty in the position of the a-beryllium primary solid-solution boundary is about 0.5 at. pct (3wtpct). Losana and Goria3 in studying the beryllium-nickel phase diagram, determined the solid solubility of nickel in beryllium by thermal analysis. They found the maximum solubility to be between 1.65 and 2.65 at. pct (10 to 15 wt pct) at 1240°C. This value decreased rapidly with decreasing temperature. In determining approximate ranges of solubilities for different elements in beryllium, Kaufmann, et al,8 reported a value of between 1.3 and 1.7 at. pct (7.9 to 10.1 wt pct) for the solubility of nickel in beryllium. The value was obtained by metallographic examination of quenched alloys and lattice-parameter measurements. However, the authors also noted a single-phase structure for a 1.7 at. pct Ni alloy (10 wt pct) on cooling from the liquid. This would indicate a higher solubility range than was reported. ~isch,&apos; in his X-ray studies of beryllium-copper, beryllium-nickel, and beryllium-iron intermetallic compounds, reports the disappearance of a second phase (Ni,Be2) in the beryllium primary solid solution at approximately 4 at. pct (20 wt pct). THEORY The analysis of concentration gradients in diffusion couples has proven to be a useful tool in determining phase equilibria.8-14 In this particular study the diffusion couples were chosen to straddle the expected composition range of the phase boundary, then heat treated at a given temperature and the concentration gradient evaluated. The composition of the phase boundary for a given temperature appears at a point of discontinuity of the composition gradient. Examples of typical phase diagrams and the concentration gradients which should be found in such systems are shown in Fig. 1. In the present work, gradients of the form of Fig. l(c) were obtained in diffusion couples made of pure beryllium and two-phase alloys of beryllium with either iron or nickel. The composition at the point where the gradient becomes discontinuous, Cs, corresponds to the solubility limit of either iron or nickel in beryllium. The analysis of the concentration gradients was carried out by an X-ra absorption method developed and applied by Ogilvie and later used by Moll13 and Hilliard.l4 It depends on the fact that the absorption of X-rays by matter is determined by the concentration and type of the various atomic species present. The relationship for the intensity, I, of a monochro-

Jan 1, 1960

By L. A. Wood, A. G. Winslow

Subsidence has occurred in several areas of the upper Gulf Coast region of Texas, although in most cases this is not evident without precise instrumental leveling. As referred to in this report, the region comprises about 7200 sq miles of the Gulf Coastal Plain and includes all or parts of the following counties: Harris, Fort Bend, Waller, Brazoria, Galveston, Liberty, Chambers, Orange, and Jefferson (Fig. 1). Topographic relief is low, ranging from sea level at the Gulf of Mexico to 300 ft or more in northwestern Harris County. In this upper Gulf Coast region, which embraces the most heavily populated and industrialized parts of Texas, industrial and municipal water supply is obtained chiefly from wells. Largest center of ground-water withdrawal is the Houston-Baytown area, where about 200 million gallons per day was pumped in 1956 for municipal and industrial use. Other large centers of ground-water withdrawal include the Alta Loma sector and the heavily industrialized Texas City area in Galveston County, where about 23 mgd was pumped in 1956. In the Freeport area in Brazoria County about 6 mgd was pumped in 1956 for city and industrial supply. In addition to withdrawals in metropolitan districts, great quantities of ground water are supplied by irrigation wells to thousands of acres of rice. These wells are widely dispersed over many miles, principally in Harris, Waller, Fort Bend, Brazoria, and Liberty counties, and effects of pumping are not so readily noticed as in the industrial and metropolitan sectors. Subsidence: Starting with the 1905-1906 line from Smithville, Tex., to Galveston, the U. S. Coast and Geodetic Survey has extended a network of first and second-order level lines throughout the upper Gulf Coast region. In 1918, when a line was run from Sinton, Tex., to New Orleans, La., a tie was made to the 1905 leveling at Houston. In 1932-1933 a line was run from Palestine, Tex., to Houston, and a good deal of leveling was carried out in the vicinity of Houston. At this time the entire network was adjusted to the Sea Level Datum of 1929. In 1935-1936 and 1942-1943 several new lines were run and considerable releveling was performed. Supplementary adjustments were made after both the 1936 and 1943 levelings in order to reduce the elevations to the Sea Level Datum of 1929. These adjustments probably masked some of the subsidence that had occurred up to that time, although a certain amount of subsidence was noticed in the 1943 leveling. When several lines in the vicinity of Houston and Galveston were releveled in 1951, the regional nature of the subsidence became apparent.&apos; Direct comparison with the 1943 leveling was possible because the datum was not changed. Comparisons with prior leveling were unreliable because of differences in the early and subsequent datums. In 1953-1954 many lines in the region were re-leveled and in 1957 the entire network, including the elevations previously determined, was readjusted to determine the changes in elevations as indicated by various levelings between 1905 and 1953-1954. In this instance the adjusted elevations were held fixed near the boundaries of the region where the bench marks seem to have remained stable. The only sea-level connection held fixed was the connection of the 1905 leveling to the 1903-1906 tidal series at Galveston. Almost the entire region has been at least slightly affected by the subsidence, some areas to a great extent. The profiles of subsidence (Fig. 2) and the map showing the contours (Fig. 3) illustrate both regional and local changes. A large area of subsidence is centered in the Houston-Baytown district, where the maximum recorded is about 2.7 ft between 1905 and 1954. This probably falls short of the actual maximum, since land surface subsided as much as 2.5 ft in the industrial section alone between 1943 and 1954. Sub-

Jan 1, 1960

By A. J. Griest, P. D. Frost, J. R. Doig

During the past 5 years, research directed toward the development of titanium alloys having improved strength-ductility relationships and heat treatability has been carried out at Battelle for the U. S. Air Force.1"3 In the course of this work, a method of heat treating ß-stabilized titanium alloys was developed which produced a wide range of useful properties.4 The heat treatment consisted of two steps: a) solution treating at temperatures in the a-ß phase region, and b) overaging at a lower temperature in the range 800°to 1100°F. Corollary to the alloy development work, research was conducted on the mechanism of the heat-treatment reaction. The investigations of Frost and co-workers on isothermal transformation in Ti-Cr5 and Ti-Mn8 alloys disclosed the existence of the transition phase, w, during the course of the decomposition of metastable ß phase. Subsequent work at Battelle7,8 &apos;and at Case Institute by Brotzen and co-workerss further clarified the nature of the decomposition process. Beta decomposition was found to proceed by the following series of reactions: 1 2 3 4 a + Ti, My (in eutectoid systems). ßo, ßr, and ßU refer to ß phase of original, enriched, and ultimate alloy contents, respectively. Omega is a transition phase having a complex structure. 10-13 Step 4, of course, occurs only in ß-eutectoid systems. This paper presents data correlating transformation behavior with mechanical properties for the following alloys: Ti-8Mn, Ti-8Mn-2A1, Ti-4Mn-4A1, Ti-6Al-4V, and Ti-4Fe. The isothermal decomposition of ß in titanium-manganese alloys of similar composition has been investigated by Frost and coworkers8 and the effect of various annealing treatments on alloys in this system has been studied by Holden, Ogden, and Jaffee.14 The compositions Ti-8Mn-2Al, Ti-4Mn-4A1, and Ti-6A1-4V, were studied in the present work in an effort to define more clearly the effect of aluminum on the response to solution and aging treatments. Ogden, Holden, and Jaffee15 have invesitgated the effect of aluminum on the response of a similar alloy (Ti-8.8Mn-2.46A1) to annealing treatments, and Luini and Lee16 have made an exploratory investigation of the heat-treatability of the Ti-4Mn-4Al alloy. The Ti-4Fe alloy was studied as an example of a moderate1y active eutectoid system. Holden, Ogden, and Jaffee 17 have studied Ti-Fe alloys and have presented some hardness data for aging at 400°C for alloys of Ti-2.56, 5.01, and 7.35 iron after quenching from the a-ß field (750°C). EXPERIMENTAL PROCEDURES The experimental procedures generally used in the precipitation-hardening study are outlined in the following sections. Departures from these techniques are noted in the discussions of the individual alloys. Table I presents the nominal and actual compositions of the alloys studied, together with the swaging and rolling temperatures. In all cases, these temperatures were in the a-ß field and the microstructures consisted of an equiaxed a-ß mixture. Melting and Fabrication—Except for the commer-

Jan 1, 1960

By F. H. Spedding

From thermal, metallographic, X-ray, dilatometric, and electrical resistance data a Phase diagram is proposed for the La-C system. TWO compounds are formed, body-centered-cubic Laz C, having a large range of solid solubility, and body -centered-tetrago-nal Lac2 . The former melts incongruently at 1415°C, and at 25OC it has an electrical resistivity about two and one-half times that of bure lanthanum. The latter melts congruently at 2356°C and at room temperature has an electrical resistivity about equal to that of bure lanthanum. The addition of carbon to La lowers the melting Point of La about 115&apos; C, raises the higher (B-Y) transfomzation about 10" C and appears to have no effect on the lower ( a-0) transformation. The addition of carbon appears to lower the oxygen content in the metal and improve the machinability; however, the tendency to oxidize is increased. Two eutectics are formed in the system. The first occurs at 2.2 pct C and melts at 806" C, while the second occurs between Lac2 and C with a melting point of2271"C. PETTERSSON,~ in 1895, was the first to prepare lanthanum dicarbide by heating the oxide with carbon in an electric furnace. He showed that this yellow, crystalline but brittle carbide had a formula corresponding to LaCz and that it reacted with water with the evolution of hydrogen and hydrocarbons and the formation of the hydrated oxide. Von Stackelberg&apos;s investigation of the crystal structure of the MCz carbides showed that the lanthanum dicarbide is of the tetragonal calcium dicarbide-type structure. He found the lattice parameters were a = 3.92 and c = 6.56.* Bredig,&apos; using X-ray methods, showed that the room-temperature form of lanthanum dicarbide is stable up to 1750 °C and that above this temperature it transformsoto a face-centered-cubic structure, a = 6.0 ± O.lA, probably of the pyrite, FeSzstruc- typ? The reported discovery of two new cerium carbides, suggested that a corresponding face-centered-cubic lanthanum monocarbide and a body-centered-cubic lanthanum sesquicarbide might exist. This paper describes work on the lanthanum-carbon system which is part of a study of the rare earth metals and their alloys now in progress in this laboratory. EXPERIMENTAL PROCEDURE Source of Materials—The lanthanum metal was prepared at the Ames Laboratory by metal1o;hermic reduction of the fluoride with calcium metal. The results of spectrographic and chemical analysis indicated the presence of 0.01 pct Y, Al, Cu, Fe, and Si; 0.02 pct Ca and Mg; 230 ppm C; and 115 ppm N. The carbon used was of two types: 1) "National Special Graphite Spectroscopic Electrodes," and

Jan 1, 1960

By S. B. Lement

THE nature of the carbides that form during the tempering of martensite is a subject of continuing controversy. The only direct methods of identification available are X-ray and electron diffraction. These methods are subject to several difficulties. Only a relatively few diffraction lines of appreciable intensity emanate from carbide phases that are formed at low tempering temperatures. Furthermore, some overlapping of carbide and matrix lines occurs. There is also the problem that numerous lines in the patterns of possible carbide phases that may be present have about the same d-spacings. Increasing the number of carbide lines and eliminating the matrix lines can be accomplished by extraction techniques. However, there is always the possibility that a change in carbide structure will occur as a result of removal from the parent matrix. Therefore, such techniques as electrolytic extraction and making extraction replicas should be checked by other methods. For identifying small amounts of carbide in a tempered martensitic matrix, electron diffraction carried out in reflection is more advantageous than X-ray diffraction. To properly prepare a specimen for reflection electron diffraction, an etchant that will selectively attack the matrix and thereby cause the carbide particles to stand in relief should be used. With an electron beam directed at a grazing angle to the specimen surface, the major contribution

Jan 1, 1960

By Schrade F. Radtke

THE law of our present industrial society is the law of the jungle. By this I mean survival of the fittest. I do not refer to man or animal or the development of superior genetic strain. Rather do I refer to one's product, one's process, or one's material of construction. Each must perform in a superior manner or it is doomed to extinction; it must be steadily improved so that it can meet the competition of ether materials, of other equipment, or other processes. We have before us the classic examples of the horse and buggy vs the automo-bile, cf silk vs nylon, of the steam locomotive vs the diesel engine; in each case, a superior product has virtually wiped out its predecessor. Furthermore, a product, process, or piece of equipment is sold on its performance, together with engineering data which define its •characteristics and performance. For the most part, the present day sales-man must deal in terms of engineering performance of his product; he must know competitive materials -their strength and limitations as well N either old fashioned salesmanship, tradition, nor custom could have saved the horse and buggy from extinction; a superior product which has been steadily and con-sistently improved won out, 'and in turn, this change-over caused a dramatic• change in our whole way of life.

Jan 1, 1960

By J. Quigley

As the outcrop mines in the West developed into underground operations, systems of ground support were gradually evolved. In the early coal mines there was little need for support except near the dirt line in portals, where stone masonry was common. Where the top was shaley or broken, native pine props with light cross bars and legs furnished enough support even in Utah&apos;s 25-ft coal seams. As depth of workings increased. roofs and backs of the same general nature as those near the surface became more and more unstable and required more and more support. Some coal airways show this tendency very clearly. From the surface down the same type of roof shows deterioration which an experienced eye can translate into a measure of depth under surface rather than change in rock characteristics. Rock bolts, developed by various companies and by the U. S. Bureau of Mines, have become an effective substitute for timber in sections of some metal and nonmetal mines formerly requiring escessive timber support, and further use of war surplus landing mats, chain link fencing, and a new punched channel developed by one of the steel companies has enabled other mines to operate deposits where costs of timber and lack of clearance for timber support would have prohibited mining. The block caving mines have made extensive use of reinforced concrete underground to achieve similar ends under difficult conditions. Steel sets are standard in many Bureau of Reclamation projects, although these are usually covered in with concrete to make the permanent structures the Bureau&apos;s reclamation projects require. But the use of steel in mining operations is limited and has been confined principally to the iron ore mines of Michigan, Wisconsin, and Minnesota. Some mines have installed used rail as posts, caps, and crossbars, but a rail section is not suited for load carrying, and used rails are generally brittle. having a tendency to fail without warning when overloaded. European mines were the first to reach the size of worked out areas and depths of cover resulting in major roof problems. The Europeans resorted to pack walls and masonry walls, in conjunction with timber arched sets. rail arches, and combination timber and rail and steel arches. The give in these pack walls and wooden blocking was supplemented by a hinge in the center of the arch. This design is called an articulated arch Through various refinements of this principle of the support giving graduallv with the load. Toussaint-Heintzmann developed the yielding or sliding arches, in which yield is accomplished by friction in the overlapping joints of the arch. This type has gained widespread acceptance in the Ruhr and Lorraine Basin and is being manufactured by Bethlehem Steel for sale in this country. In North America the anthracite mines in Pennsylvania, followed by certain iron ore mines in upper Michigan and Canada, were the first to employ these arches to any extent. The practice was later adopted by Kennecott at Ruth, Nev., and by others. Despite high initial cost, the use of these arches is growing in many parts of the country because of their suitability in heavy ground. In its present form of manufacture the yield-able arch consists of open U-shaped rolled section with heavy beads on the edge. The open edge of the U is placed toward the wall. The section nests in another section of the same dimensions, and an arch can be built up from rolled radii and tangents of various weights and lengths. Sections are fastened together by U bolts and saddles. The lap on the joint varies from 12 to 24 in., and ordinarily the bolts are tightened with a 1-in. drive air wrench. The arches are spaced with channel struts held by J bolts and saddles. Sections can also be obtained that are composed of various combinations of radii and tangents and true circles. The joints can be placed to bear against anticipated loads and asymmetrical loads imposed by dipping strata. In the arches now being manufactured clearance widths up to 19 ft are obtainable in weights of sections from 9 to 30 lb per ft. The circular cross sections are available in the same weights ranging from 8 to 16 ft diam. At present most of the arches sold are supplied only in carload lots. It is hoped that demand will grow so that distributors can stock various weights and sections to give small operators a chance to try this new type of rock support under their own particular conditions. Several excellent papers have discussed the properties of various sections now manufactured, the dimensions of the sets obtainable, and their application under widely differing conditions. The present article will describe the methods and results of a special use of the arches at Kaiser Steel mine No. 3. Sunnyside, Utah. Problem at Mine No. 3 : In 1953 Kaiser Steel Corp. laid out Sunnyside mine No. 3 to recover coking coal left by the previous operator, Utah Fuel Co.. below workings that had been abandoned in 1928. Two seams had been worked, the upper and lower, separated by 30 to 42 ft of rock. Approximately 10 million tons of coal had been extracted from this area some 3000 ft down the itch from the outcrop to a 1500-ft depth of cover. The mine had been opened by slopes in both upper and lower seams. Sometime in the late 1920&apos;s the lower slope

Jan 1, 1960

By J. W. Gregg, P. M. Dranchuk, D. L. Flock

"From preliminary investigations it has been observed that although evaporation losses may be estimated by comparing single values of certain physical properties of crude oils and their evaporation residues, such techniques possess little accuracy unless both the evaporation process and the variation of the property as a function of the process are completely known. The accuracy of estimation may be increased somewhat through the comparison of property mid-per-cent curves. Further increases in accuracy are possible if bottoms yield •curves rather than mid-percent curves are used. The use of both the mid-percent and bottoms yield curves however involves a prohibitive amount of effort in most cases. Examinations of distillation bottoms from Hempel type distillations carried to end points just short of the cracking point have indicated that these bottoms are not appreciably affected by the evaporation process. It was further observed that bottoms of identical API gravity, obtained from a crude oil and its evaporation residues behave as if they were pure components which were unaffected by evaporation. Based on these observations Hempel distillation bottoms of equal API gravity were obtained for a crude oil and its various evaporation residues from API gravity bottoms yield curves. The volume percent of these bottoms in the crude oil and its residues were used to calculate the evaporation losses suffered by the crude in order to yield the various residues. The results indicate that, although further refinements in technique are required, it is possible to calculate evaporation losses with an accept-able degree of accuracy through the use of this method."

Jan 1, 1960

By J. F. Tavernelli, L. F. Coffin

The deformation and fracture characteristics of eight metals subjected to fully reversed cyclic strain ranging from 0.2 to 50 pct were investigated at room temperature. Strain-hardening characteristics unique to the interna1 structure of a particular metal were found. Complete removal of the strain-hardening effects resulting from prior deformation was brought about by subsequent cyclic strain. Further support for the validity of the inverse relationship between the plastic strain range and the square root of the number of cycles for failure is given. THE resistance of materials to cyclic plastic strain is of interest both from a fundamental and practical point of view. It is now a well-accepted fact that fatigue failure in metals is a consequence of the localized slip deformation which occurs within the individual crystals of metal.&apos;-&apos; Hence the failure process should be strongly dependent upon the magnitude of the gross cyclic plastic deformation of the metal under conditions where this is a measurable quantity. Therefore, an experimental investigation of metals in which the cyclic plastic strain is the independent variable should shed new light on some of the basic aspects of the problem. From the practical point of view, there are many uses for information relating to the cyclic strain resistance of metals. One is the case of thermal stress fatigue where fatigue failure can occur as a consequence of a com- paratively few cycles of thermally induced mechanical deformation. Another is the mechanical working of metals where large cyclic strains are employed. In recent years several publications have appeared relating to the cyclic-strain resistance of metals,8-11 dealing mostly with the fracture aspects where the temperature is cycled simultaneously with the mechanical strain. Some work has been reported on the cyclic-strain resistance of metals at constant temperature, again oriented more toward the fracture aspects of the problem than the deformation aspects. 12-16 The present research investigation was undertaken to obtain information regarding the deformation characteristics of several metals whose structure-property relationships were simple and straightforward under conditions of both cyclic and monotonic strain. It has been shown for example that under cyclic-strain conditions some materials will strain harden, while other materials, particularly cold-worked structures, strain soften and these effects required further clarification.8,17-19 It was also de-

Jan 1, 1960

By R. H. Singleton

ThE purpose of this investigation was to determine the effect of cerium upon the nonmetallic inclusions found in cast and wrought steel containing various amounts of sulfur, oxygen, and nitrogen. Interest of the Physical Metallurgy Laboratory of the Watertown Arsenal Laboratories in this type of research was stimulated by the reports from industry that rare-earth metals imparted beneficial effects upon the mechanical properties of steel, but that the mechanism was not understood. Berry and Dorvel&apos; found that misch metal improved the impact properties of aluminum-killed cast steels. They reported that the rare earths modified the intergranular-film type nonmetallic inclusion, present with aluminum as the sole deoxidant, to a randomly distributed globular type. Lilliequist and Mickelson2 observed the improvement of ductility and toughness of quenched and tempered cast steels through rare-earth additions. They also observed the change from angular to duplex inclusions when rare earths were present. They con-

Jan 1, 1960

By J. B. Evans

"NORMALLY the duties of the exploration engineer and geologist cover the initial, and possibly, the most important phase of mining property evaluation; that phase being the presentation of an opinion of the property's ore reserve potential in terms of tonnage and grade. The prime objective of this pa-per is to outline one method of bridging the wide gap that lies between a know ledge of a property' s tonnage and grade potential and an appreciation of the value of that property in dollars and cents.THE PRESENTATION OF PROPERTY EVALUATIONThe engineer engaged on a mining property evaluation, regardless of whether he be an independent consultant, or a company employee, has as his goal, the presentation of his appreciation of the property's potential value or worth within terms of reference acceptable to his principal.To furnish a complete evaluation report, the evaluator must firstly study all aspects pertaining to the particular property under consideration, then present his appreciation of the property's worth in some tangible form. The ultimate presentation is one giving a Present Value of the pro pert y in terms of monetary exchange. Such an idealistic presentation is not always possible; typical preventives being -insufficient reliable information, limited time, Jack of ability and absence of definite direction."

Jan 1, 1960