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By T. N. McVay, E. E. Creitz

Rather large amounts of titanium minerals and some zircon and monazite are being recovered from dune sands about I. miles west of Jacksonville Beach, Fla. The Mining Branch of the Bureau of Mines, Southern Experiment station, has been interested in developing additional large deposits of similar sands in other areas of Florida. The results of a field study have been published1 concerning the sands occurring on Trail Ridge which runs north and south about 30 miles southwest of Jacksonville. This investigation was undertaken in order to identify the opaque titanium minerals occurring in Trail Ridge and because of the economic importance of Florida titanium minerals. Nature of the Problem The minerals present in the heavy fractions (sp gr > 2.94) of the sands are principally opaque minerals; staurolite, zircon, sillimanite, tourmaline, kyanite, rutile, a small amount of corundum, traces of the zinc spinel gahnite and garnet. Epidote, monazite, hornblende and ti-tanite are present in other dune sands but these minerals were not noted in the samples collected on Trail Ridge. All of the minerals except those which are opaque can be readily identified by the usual petrographic methods. However, Opaque minerals cannot be examined satisfactorily by transmitted light. Polished sections of the opaque-mineral grains were examined but these sections did not furnish useful information. Consequently, it was necessary to use means other than the usual petrographic methods to identify them. Previous Investigations of Heavy Minerals in Florida Sands Martens2 has described the heavy minerals in the Florida beach sands and has classified the opaque minerals as ilmenite with minor amounts of leucoxene. Miller3 studied a number of sands collected by Ross and Mertie in Florida. He states that the material from the Florida beach and dune sands that commonly has been called ilmenite has essentially the chemical composition of the material that has been called arizonite.4 The x ray diffraction patterns of several samples indicated that the supposed ilmenite is essentially amorphous, with only weak lines corresponding to ilmenite, and hence the material is unlike the type of arizonite from Arizona. Opaque Titanium Minerals Rutile is essentially titanium dioxide. However, as pointed out by Dana,5 important amounts of Fe+2 and Fe+3 as well as Cb and Ta are reported in some analyses.

Jan 1, 1949

By B. F. Decker, D. Harker

The recrystallization reaction in OFHC and spectroscopically pure copper has been followed by X ray diffraction determinations of the amount of material with the cold-worked and recrystallized textures in specimens which had been given various heat treatments. The heats of activation for recrystallization are found to be: 29.9 kcal per rnol for OFHC copper and 22.4 kcal per rnol for spectroscopic copper. A reliable and speedy method for measuring the amount of recrystallized material in a piece of rolled metal, together with a new scheme for low temperature heat treatment, have made possible a determination of the activation energy for recrystallization in rolled copper. This method for studying recrystallization rates is different from others reported in the literature.' Oxygen free, high conductivity copper—OFHC copper—of purity 99.98 pct gave an activation energy for recrystallization of 29.9 kcal per mol with recrystallization data taken in the temperature range 208-245°C. Copper of purity 99.999 pct from the American Smelting & Refining Co. gave an activation energy for recrystallization of 22.4 kcal per mol with recrystallization data taken in the temperature range 43-135°C. The great change in activation energy for recrystallization as the small amount of impurity in the metal is decreased suggests that the motion of grain boundaries is conditioned by the impurities which must be concentrated in them. Thus the OFHC copper recrystallizes with an activation energy of the order of magnitude to be expected for the diffusion of the kind of impurities likely to be present. The high purity copper, on the other hand, recrystallizes with a much lower activation energy, in accord with the notion that the grain boundaries need not wait for the impurities to diffuse with them. Copper when strongly cold-rolled has a well-defined crystallite texture which can be described by saying that the [111] direction of the face- centered cubic crystals is aligned approximately in the cross-rolling direction and that faces of the form {110} lie approximately in the rolling plane. When such rolled copper is completely annealed the crystallite texture is quite different: the [loo] direction is in the cross-rolling direction and faces of the form (100) are in the rolling plane. At intermediate stages of annealing, the copper contains both textures. If a Geiger counter X ray diffraction spectrometer is set up so as to measure the intensity of the (200) Bragg reflection from the rolled surface of a piece of copper strip, this intensity increases from a very small value in the cold-worked state to a maximum as the specimen is annealed. The same would be true for (200) reflections from planes normal to the rolling or cross-rolling directions. In view of this fact, the amount of material in the copper which has recrystallized can be measured by comparing the intensities of one of these reflections just mentioned with the intensity from a similar specimen after complete annealing. In much the same way the intensity of (111) reflections from planes normal to the cross-rolling direction could be used to measure the amount of unrecrystallized material in the specimen. In the work to be described here the amounts of recrystallized and unrecrystallized material in partly annealed rolled copper specimens were determined in this way. Experimental Procedure Samples of oxygen free high conductivity (OFHC) copper, cold-rolled 99.7 pct to 0.002 in. thickness, were subjected to heat treatments for various chosen times at four different temperatures, and high purity copper samples, cold-rolled 98.0 pct to 0.0015 in. thickness, at six different temperatures. Each sample, after treatment, was placed in an orientation sample holder for use with a Geiger counter X ray spectrometer and a reading was taken of the intensity of the (200) reflection from planes perpendicular to

Jan 1, 1951

By R. B. Fuller

DURING the summer of 1949, the United Nations Scientific Conference on the Conservation and Utilization of Resources met at Lake Success. As summed up by one writer, the purpose was: "That everyone will try to learn how to feed more people from an acre of land." That objective is a stimulus to the phosphate rock industry as well as other industries.

Jan 8, 1951

By G. Kimmel, A. Bar-Or

The rate of nucleation and the rates of both lateral and longitudinal growth of martensite plates (needles) in b—a transformation were determined as a function of temperature, in various U-Cr alloys. The activation energies for nucleation and both modes of growth were calculated from the experimental results. The identical values for lateral and longitudinal growth clearly indicate that both are controlled by the WHITE,' Mott and Hines and Holdeen3 showed that characteristic martensite plates (needles) appear in U-Cr alloys during the transformation 8 —0 in the lower temperature range (up to -300°C). Holden pointed out that the rate of growth of the individual martensite plates under isothermal conditions is same mechanism. Lomer's suggestion that single-atom movement over subatomic distances controls the specially slow growth of martensite receives further support from the present kinetic study, which shows that the growth rate can be described quantitatively by known formulas for the growth rate in processes involving single-atom movement. very slow, and suggested that this is due to the slowness of the relief of the stresses engendered during the growth of the individual plates. lomer4 attributed the slow growth to the complexity of the atomic adjustment at the growing interface b/(u. In the present work the rates of nucleation and growth of martensite plates in U-Cr alloys were studied by direct observation, in order to elucidate the mechanism which controls their characteristic slow growth.

Jan 1, 1968

By Michel T. Halbouty

The area for which oil and gas development is reported for 1938 in this paper is larger than that covered by the report for 1937, in that besides Duval, Jim Hogg, McMullen, Starr, Webb and Zapata Counties, comprising the Laredo district, this paper also includes the South Corpus Christi district, which is composed of the following counties: San Patricio, Nueces, Jim Wells, Kleberg, Kenedy, Brooks, Willacy, Hidalgo and Cameron, all heretofore included in A.I.M.E. Gulf Coast reports. In the map, Fig. 1, the area known as South Texas is represented by the counties south of the heavy black line. Production in the South Corpus Christi district, which covers an area that extends inland for 50 miles and follows the coast line, is primarily in zones ranging from the Catahoula, through the Frio sands, into the Vicksburg horizon. General exploration is done mainly with geophysics because in this district production is directly dependent upon structural conditions. In the Laredo district most of the production is from sand lenses; therefore, because these shallow sand lenses represent old shore lines which are monoclinic in character, the most satisfactory method of exploration in the Laredo district is drilling. This type of production centers around Duval County and follows a northeast-southwest trend along the Mirando district. Although drilling operations showed a decline from the preceding year, 1938 was highly successful as far as new discoveries and developments were concerned, and results of the year's operations should have an important effect on the near future trend of exploration and drilling. Besides the discovery of several new fields and many new sands in established fields, 1938 saw the discovery of a new Vicksburg sand trend and the first marine drilling off the South Texas Gulf Coast. Many new fields were discovered during the year, but only a few were subjected to an extensive drilling program. Several already established fields, especially in the Laredo district, received a large amount of drilling as new sands and extensions enlarged the producing areas, a

Jan 1, 1939

By Michel T. Halbouty

The area for which oil and gas development is reported for 1938 in this paper is larger than that covered by the report for 1937, in that besides Duval, Jim Hogg, McMullen, Starr, Webb and Zapata Counties, comprising the Laredo district, this paper also includes the South Corpus Christi district, which is composed of the following counties: San Patricio, Nueces, Jim Wells, Kleberg, Kenedy, Brooks, Willacy, Hidalgo and Cameron, all heretofore included in A.I.M.E. Gulf Coast reports. In the map, Fig. 1, the area known as South Texas is represented by the counties south of the heavy black line. Production in the South Corpus Christi district, which covers an area that extends inland for 50 miles and follows the coast line, is primarily in zones ranging from the Catahoula, through the Frio sands, into the Vicksburg horizon. General exploration is done mainly with geophysics because in this district production is directly dependent upon structural conditions. In the Laredo district most of the production is from sand lenses; therefore, because these shallow sand lenses represent old shore lines which are monoclinic in character, the most satisfactory method of exploration in the Laredo district is drilling. This type of production centers around Duval County and follows a northeast-southwest trend along the Mirando district. Although drilling operations showed a decline from the preceding year, 1938 was highly successful as far as new discoveries and developments were concerned, and results of the year's operations should have an important effect on the near future trend of exploration and drilling. Besides the discovery of several new fields and many new sands in established fields, 1938 saw the discovery of a new Vicksburg sand trend and the first marine drilling off the South Texas Gulf Coast. Many new fields were discovered during the year, but only a few were subjected to an extensive drilling program. Several already established fields, especially in the Laredo district, received a large amount of drilling as new sands and extensions enlarged the producing areas, a

Jan 1, 1939

By C. Kolm, E. P. Warekois, S. A. Kulin

MUCH insight has been gained into the nature of the cold-worked state of metals in recent years through the use of modern X-ray techniques. These methods have revealed the existence of stacking faults together with regions of high internal strain and have provided means of measuring the atomic perturbations in plastically deformed metals. In view of the recent increased interest in the solid state, it is desirable to extend these techniques to the study of lattice imperfections introduced into semiconductors during plastic deformation. It is of particular interest to compare the state of imperfection sustained by metallic bonding with that sustained by the covalent bonding found in semiconductors. A knowledge of the imperfections which can exist in semiconductors is important from both a theoretical and a practical point of view since they can greatly influence many of the physical properties. In order to determine the possible existence of stacking faults in covalently bonded structures, precise measurements were made of the diffracted peak positions of plastically deformed germanium, gallium antimonide, and indium antimonide. These measurements were based on the theoretical treatment of Paterson1 and are similar to those employed by Warren and warekois2 in their studies of deformed a brass. In addition, diffraction peak profiles were measured on the annealed and plastically deformed materials in order to obtain information concerning the distribution of internal strains through the use of the Fourier methods developed by Warren and Averbach.3 EXPERIMENTAL PROCEDURES AND TECHNIQUES Because of the room-temperature brittleness of the semiconductors studied, it was necessary to plastically deform the materials at elevated temperatures. The brittle-ductile transition temperature ranges of GaSb and InSb are sufficiently low to permit hot-filing operations. Therefore, high-purity, polycrystalline GaSb and InSb were filed in an argon atmosphere at 400' and 300°C, respec-

Jan 1, 1959

By J. D. Davis, A. C. Fieldner

The older coal chemist had a much simpler conception of coal than we have today. To him coal was a mineral composed essentially of carbon, hydrogen, oxygen, nitrogen, sulfur, ash, and water, in various proportions. His studies on the constitution of coal were directed along the conventional lines of proximate and ultimate chemical analyses and making deductions from these data without any real appreciation of the fact that coal is a conglomerate of various chemical compounds, including many of the most complex structures known to organic chemistry. The view of the modern coal chemist is well expressed by Franz Fischer,' who says that while proximate and ultimate analyses are important both from the scientific and technical point of view, they tell the chemist no more concerning the number and kinds of chemical compounds that constitute coal than the reader would learn of the contents of a book if told that the printed contents consisted of 15 per cent. of the letter "e," 5 per cent. of the letter "n," 1 per cent. of the letter"g," 4 per cent. of the letter "b," etc. As the reader must have the grouping of letters into words and words into sentences, so the chemist must have the grouping of atoms into molecules and the proportion of each molecular compound in the coal aggregate before he acquires an adequate knowledge of the constitution of coal. Modern investigators2 are laying the foundation of a new chemistry of coal based on the biochemistry of plants and the chemical changes involved in processes of fermentation and decay. As

Jan 1, 1925

By Kenzo Ikeda

The Kosaka smelter is situated in the extreme northern end of Hondo (the main island of Japan) 15 mi. east of Odate, on the government railroad, to which it is connected by a private railway. It contains ten blast furnaces having a maximum daily capacity of 1600 short tons of ore, conducting a slow pyritic smelting entirely without coke or limestone, and with a charge carrying over 50 per cent. of briquetted and agglomerated fines. The matte (35 per cent. Cu) is blown in two basic-lined barrel converters, the blister copper (98.8 per cent. Cu) being cast at once into anodes. The adjoining refinery contains 600 tanks with a maximum capacity of 1300 tons of cathodes per month, the byproducts being gold, silver, and bismuth. At present, working at about half capacity, the whole plant consumes 2000 kw. of hydro-electric power, and employs 850 men and women. The ores are derived from two principal sources: The relatively new Hanaoka mine, 20 mi. from the smelter, yielding copper pyrites by underground mining, and the old Kosaka open-cut mine, 1 1/2 mi. from the smelter, yielding three different ores: (a) kuromono, a compact finegrained mixture of barite (32 per cent.), zinc blende, galena, and pyrite, the whole carrying about 2.5 per cent. Cu; (6) cupriferous pyrites with 2.4 per cent. Cu; (c) siliceous ore with 2 per cent. Cu. The Hanaoka ore now constitutes approximately one-half of the charge, almost replacing the Kosaka kuromono which was the ore chiefly smelted until 1913.'

Jan 1, 1923

By Kenzo Ikeda

The Kosaka smelter is situated in the extreme northern end of Hondo (the main island of Japan) 15 mi. east of Odate, on the government railroad, to which it is connected by a private railway. It contains ten blast furnaces having a maximum daily capacity of 1600 short tons of ore, conducting a slow pyritic smelting entirely without coke or limestone, and with a charge carrying over 50 per cent. of briquetted and agglomerated fines. The matte (35 per cent. Cu) is blown in two basic-lined barrel converters, the blister copper (98.8 per cent. Cu) being cast at once into anodes. The adjoining refinery contains 600 tanks with a maximum capacity of 1300 tons of cathodes per month, the byproducts being gold, silver, and bismuth. At present, working at about half capacity, the whole plant consumes 2000 kw. of hydro-electric power, and employs 850 men and women. The ores are derived from two principal sources: The relatively new Hanaoka mine, 20 mi. from the smelter, yielding copper pyrites by underground mining, and the old Kosaka open-cut mine, 1 1/2 mi. from the smelter, yielding three different ores: (a) kuromono, a compact finegrained mixture of barite (32 per cent.), zinc blende, galena, and pyrite, the whole carrying about 2.5 per cent. Cu; (6) cupriferous pyrites with 2.4 per cent. Cu; (c) siliceous ore with 2 per cent. Cu. The Hanaoka ore now constitutes approximately one-half of the charge, almost replacing the Kosaka kuromono which was the ore chiefly smelted until 1913.'

Jan 1, 1923

US 4,185,193-Method of assaying the vicinity of a borehole for uranium ore or thorium ore. A pulsed neutron source IS operated to irradiate the earth formations with fast neutrons. A detector responds to the delayed fission neutrons emitted by the ore as a measure of ore concentration and to the delayed neutrons from oxygen-17 as a measure of the neutron output of the source. The measurement of ore concentration is corrected In accordance with the measured changes in the neutron output of the source. R L. Caldwell, assigned to Mobil Oil Corp. Jan. 22, 1980 4 pp (250-269). Filed: 5-18-78 (906,907).

Jan 1, 1982

E. O?C. Acker Truman H. Aldrich John H. Allen W. Lawrence Austin W. S. Ayres David Baker Andrew A Blair Walter M. Brodie H.H. Burden Charles Butters

Jan 1, 1936

By Mowry Bates

THE following example of the practical application of engineering geology is of interest in that it demonstrates the advantage of keeping accurate records of all wells, whether drilled by one's self or by others, together with the advantage gained by gathering such data during the process of development. The fault described was found in the autumn of 1915, during the hurried development caused by the discovery of the famous Gusher Bend pool in Red River Parish, Louisiana. The writer was at the time employed by one of the operating companies as geologist, and the example is a portion of the routine work. LOCATION The oil fields of northern Louisiana and east Texas are located in Caddo, Bossier, De Soto and Red River Parishes, Louisiana, and Marion County, Texas. A very narrow strip of the eastern portion of the latter is productive. The producing oil pools are known as the Caddo Field, in the northern part, and the De Soto-Red River Field, in the southern. The two fields are 60 miles apart. There are several gas fields between then, but no important supply of oil has been found, though there are several producing wells in the Anona chalk, locally called the chalk rock, in the Elm Grove gas field in Township 16 North, Range 11 West (see Plate 1).

Jan 5, 1918

Executive JOHN R. SUMAN, Chairman PAUL D. MERICA, Vice-Chairman CHESTER A. FULTON W. M. PEIRCE H. Y. WALKER Finance H. T. HAMIL'T'ON, Chairman ERLE V. DAVELER HENRY KRUMB Admissions FELIX E. WORMSER, Chairman GEORGE D. BARRON, Vice-Chairman PHILIP KRAFT EDWARD MEAGHER CLYDE E. WILLIAMS

Jan 1, 1941

By Martin Weinstein

A technique is described for preparing finegrained lead telluride by ultrasonic agitation of a solidifying melt. Material prepared by this technique is dense and chemically homogeneous. N-type PbTe, containing 0.03 mole pct PbIz, has been made and its thermoelecCric Properties have been measured as a function of temperature. For comparison, the properties of similarly doped PbTe made by cold pressing and sintering, and by extrusion, have also been measured. The ultrasonically prepared material compares favorably with the others in its thermoelectric-efficiency factor. Comparison of compressive-flow curves for the three kinds of PbTe show that the ulhasonically prepared material has much superior ductility. The cleavage strength of the ultrasonic material is related to the grain size, D, by the Petch relation:Extrapolation to infinite grain diameter yields a fracture strength of 5000 psi for single-crystal PbTe. WHEN metals and semiconductors solidify in a mold they normally assume one of three cast structures illustrated in Fig. 1.' Solidification in a casting starts at the mold walls where a large number of fine crystals of random orientation can be nucleated to form the chill zone. Because of the anisot-ropy of the growth rate, those crystals whose direction of maximum linear growth is parallel to that of the heat flow grow faster and crowd out the crystals of less favorable orientation. A second zone, having a preferred orientation, called the columnar zone, thus forms adjacent to the chill zone. The speed of growth of the columnar grains will depend, in the case of limited undercooling of the melt, on the rate at which heat can be abstracted. The columnar zone can extend to the center of the casting, Fig. l(a), but it is frequently followed, in solid-solution alloys, by another zone of equiaxed randomly oriented grains in the central portion of the casting, Fig. l(b). The equiaxed structure in Fig. l(c) represents the completely grain-refined case where the equiaxed grain size is small. The third type of structure is the most desirable because it imparts a somewhat higher strength for all except high-temperature applications, it reduces segregation of the doping constituent, and it reduces the possibility of hot tearing (the separation of grains due to the melting of a low-melting point constituent in the grain boundaries). In order to obtain fine-grained castings, the nu-cleation frequency must be increased and grain growth must be restricted. Various techniques have been employed for obtaining this end, namely: rapid cooling, vibration, and inoculation of the melt. The success of these techniques depends upon the characteristics of the metal species and on factors controlled by heat transfer through the crucible walls. Recent studies2" have shown that the application of ultrasonic energy to the solidifying ingot is an extremely powerful tool in the improvement of the crystalline structure of metallic castings. Both the mechanical properties and homogeneity of the ingots are improved. Ultrasonic oscillations may affect the crystallization process by 1) permitting subcritical nuclei to agglomerate and thus form nuclei of sufficient size to cause crystallization, 2) changing the state of surface adsorption of various catalysts found in the liquid melt, 3) breaking pieces of solid from the solidified surface near the supercooled region thereby increasing the number of possible nuclei, 4) causing temperature fluctuations to occur in certain parts of the melt thereby increasing the supercooling at specific points in the liquid, and 5) decreasing the critical nucleus size by increasing the pressure at specific points in the melt.' Various investigators have concluded that the effectiveness of the ultrasonic oscillations results from cavitation which disrupts the growing solid-liquid interface The present paper describes the application of ultrasonic oscillations to the crystallization of the semiconductor N-type PbTe. The purpose of this study is to prepare crystalline

Jan 1, 1964

By A. Steiner, K. L. Komarek

Activities of aluminum in solid Ni-A1 alloys have been determined between 20 and 60 at. pet Al and 1200" and 1400°K by an isopiestic method in which nickel specimens, heated in a temperature gradient, are equilibrated with aluminum vabor in a closed all-alumina system. The activity of aluminum shows a strong negative deviation from Raoult's law at low concentrations but increases by three orders of magnitude within the ß(NiAl) phase. The partial molar enthalpy and entropy of mixing are negative. Using Wagner and Schottky's theory of ordered compounds, a degree of disorder of 4 x 10 -4 for NiAl and 1.25 X 10-2 for FeAl has been calculated THE Ni-A1 system has been studied by a great number of investigators, and the results, as far as the phase diagram is concerned, have been compiled by Hansen.1 The phase boundaries from 0 to 50 at. pet Ni are well-established. At higher nickel contents the boundaries are still in dispute and an additional phase, A12Ni3, has been reported.' The phase diagram is dominated by a very stable high-melting compound, NiA1, with a relatively wide range of homogeneity. Heats of formation of solid alloys have been determined calorimetrically by Oelsen and Middel3 from 20 to 95 at. pet Ni and by Kubaschewski4 from 25 to 80 at. pet Ni. According to the most recent compilation5 no other thermodynamic investigations have been reported for the Ni-A1 system. Due to the corrosive nature and the low vapor pressure of aluminum, a method has been employed for determining activities of aluminum which was previously developed for the Fe-A1 system.= Nickel specimens, heated in a closed evacuated alumina system in a temperature gradient, were equilibrated with aluminum vapor from a source within the system kept at constant temperature. After complete equilibration the specimens were analyzed and activities calculated from the known vapor pressure of aluminum. APPARATUS AND EXPERIMENTAL PROCEDURE Materials. The nickel specimens were made from wafers of electrolytic nickel (International Nickel Corp.) of 99.99 pet purity which were rolled to a 0.001-in.-thick foil by Driver-Harris Co. and to a 0.005-in.-thick sheet in our laboratory. The aluminum (Aluminum Corp. of America) had a purity of 99.99+ pct. The alumina tubes and crucibles were made of impervious recrystallized alumina with an alumina content of 99.7 pet (Triangle RR, Mor-ganite Inc.). Experimental Procedure. Annular specimens were punched from the sheet, the punching burrs removed, and the specimens degreased in carbon tetrachloride and acetone and weighed on a micro-balance to within an accuracy of ±0.01 mg. The specimens were positioned with alumina spacers along an alumina tube, and the positions measured. Aluminum metal was machined into cylindrical shape, and placed into an alumina crucible. The tube with the specimens was then inserted into a hole drilled into the aluminum metal. An alumina tube with its closed end at the top was slipped over the specimens so that its lower end fitted snugly into the alumina crucible. The assembled reaction tube was inserted into a mullite tube with a water-cooled brass head which had an opening for a quartz thermocouple protection tube and a metal-to-glass connection to a conventional vacuum system. A Pt-Pt 10 pet Rh thermocouple could be raised and lowered in the quartz tube which was placed along the outside of the alumina reaction tube. The mullite tube was heated by two separately controlled resistance-tube furnaces so that in the experimental temperature range an over-all temperature gradient of approximately 150o to 250°C could be imposed on the reaction tube. The position of the mullite tube was adjusted so that the surface of the aluminum metal was always at the temperature minimum. The reaction tube was thoroughly evacuated before and during slowly heating the assembly up to the melting point of aluminum. A pressure of less than 2 µ (Hg) was maintained during an experiment. Once the aluminum had melted, it isolated the contents of the alumina tube from the surroundings. Several times during an experiment the temperature gradient was carefully measured. An experiment lasted from 3 to 6 weeks and it was terminated by air cooling the evacuated mullite tube. For further details of the experimental procedure the paper on the Fe-A1 system6 should be consulted.

Jan 1, 1964

By R. W. Heckel

The growth and shrinkage rates of second-phase particles of various size distributions are analyzed in terms of five mathematical models. These models apply to various forms of diffusion-controlled growth (one model) and interjace-controlled growth (four models). The expression for diffusion-controlled growth assumes local equilibrium at the interface between the second Phase and the matrix and through the choice of the proper flux area perrnits the definition of minimum diffusion-controlled growth kinetics. The interface-controlled kinetics models consider the situations where the rate-controlling step occurs at either the interlace undergoing solution or the interface undergoing deposition. In addition, each of these interface-controlled kinetics models is analyzed for interface reaction rates which are independent of the thermodynamic activity gradient across the interface or proportional to the gradient. THE variation of the size distribution of second-phase particles in a solute-saturated matrix has been a stimulating topic for many years. Research has been carried out in this area for situations where the matrix was either liquid or solid. It is well-understood that the over-all process results in an increase in the average particle size, a decrease in the total number of particles per unit volume, and a net decrease in surface area. Greenwood1 has presented a mathematical model based upon the mass balance existing between growing and shrinking particles. His analysis is stated in terms of Fick's First Law using concentration gradients set up between particles of different size as a result of the effect of surface curvature on solubility. Greenwood's analysis indicates that the mean particle size should increase approximately as the cube root of time. Asimow2 has shown that several of the simplifying assumptions employed by Greenwood may be eliminated from this diffusion-controlled model with little increase in complexity. Lifshits and Slyozov3-5 have also considered the growth-shrinkage problem involving diffusion-controlled kinetics. Their analysis was extended to include the effects of interacting particles ("kinetic approximation"), particle shape, and elastic strains. These authors also show that the mean particle size varies as the cube root of the reaction time. wagner6 has formulated expressions for both diffusion-controlled kinetics and interface-controlled kinetics in the growth-shrinkage problem. Wagner's diffusion-controlled kinetics is based upon the same form of mass balance using Fick's First Law as used by others and is shown to be applicable to situations where kr >> D (k is the interface reaction constant, r is the particle radius, and D is the diffusion coefficient). This analysis also yields a mean particle size which varies as the cube root of time, in agreement with other workers. Wagner also developed interface-controlled kinetics to handle kr « D. This model was based upon the fact that the interface reaction rate is proportional to the interface area. Wagner assumed that the rate was also proportional to the thermodynamic activity difference, ?a, existing across the interface. Thus, the specific reaction rate at the surface of radius r was defined as k • 4nr2 . ?a. It is the purpose of the present paper to reconsider the processes of diffusion-controlled growth and interface-controlled growth in the variation of particle-size distributions as a function of time at constant second-phase volume. The analyses are formulated in a manner which permits data obtained

Jan 1, 1965

By John W. Cloud

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

Jan 1, 1881

By Paul A. Farrar, Harold Margolin

The system Ti-Cr has been re investigated From 40 to 100 pct Cr. The high-temperature modification of TiCr, was found to exist in the temperature range from 1365 where it terminates in the eutectoid reaction TiCr,(TI)* — HE chromium-rich region of the Ti-Cr system was investigated by Vogel and Wenderott,' Mc Quillan,' Van Thyne et dl.,' and Cuff Duwez and Taylor determined the crystal structure of the low-temeperature modification of TiCr, to be fcc a = 6.943A and Levinger' discovered the existence of a second (high-temperature) modification of TiCr, and determited its crystal structure to be hexagonal a = 4.932A, c/a = 1.617i. No information was obtained as to the temperature range over which each modification of TiCr? existed; therefore the present investigation was initiated. I) Experimental Techniques Alloys employed for the delination of this system were prepared from iodide titanium and high-purity chromium. The purity of these materials is as follows: Iodide titanium: purity 99.99 pct; major impurities—carbon 0.0001 pct; oxygen 0 to 0.002 pct; nitrogen 0 to 0.002 pct; silicon 0 to 0.005 pct; manganese 0.001 pct; copper 0.001 pct (Foote Mineral Co., Lot 609-29). Chromium #1: metallic purity 99.997 min.; interstitial content—oxygen 0.27 to 0.46 pct; hydrogen 0.028 to 0.038 pct; nitrogen 0.0002 pct (Ave-quipo Inc.). Chromium #2: purity 99.9 pct; major impurities—carbon 0.01 pct; oxygen 0.013 pct; nitrogen 0.02 pct; silicon 0.01 pct; sulfur 0.03 pct; iron 0.01 pct (Fulmer Research Institute Ltd.). A total of sixteen alloys of thirteen different compositions was prepared in the range from 40 to 95' *All percentages are given in weight percent. pct Cr. The compositions of the alloys prepared were as follows: Ti-40, 45, 50, 60, 62, 64, 66, 68, 70, 80, 85, 90, and 95 pct Cr. Two buttons were prepared of the 66, 90, and 95 pct Cr alloys. The 40 pct Cr and one of the 66 pct Cr alloys were prepared from the chromium # 2. All the other alloys were prepared from chromium #1. The alloys were arc-melted as 25-g buttons in a copper-hearth glass-walled furnace7 under an inert atmosphere of high-purity helium. The alloys were sintered at 250 amp and melted twice at 350 amp for 30 sec with the buttons being turned over between melts. Weight losses during melting were determined and in the range 45 to 68 pct Cr they were found, in all cases, to be less than 1.25 pct of the total alloy weight. A number of the high-chromium alloys shattered during cooling from either the first or second melt, which made the weight loss considerably larger than usual. The 70 and 80 pct alloys lost approximately 5.7 pct of their total weight, the 85 pct alloys 1.5 pct, the 90 pct alloy 2 pct, and the 95 pct alloy 3 pct. However, it is felt that the actual composition of the alloys in this region is probably within approximately 1 pct of the intended composition, as a large portion of the material lost was that due to shattering after melting. Nominal compositions were therefore used in plotting data and referring to the alloys. The alloys were cut into specimens, wrapped in molybdenum sheet, and encapsuled in argon-filled quartz or Vycor tubes for heat treatment. The heat-treatment times and temperatures are given in Table I. The specimens were quenched in iced brine (I.B.Q.) following heat treatment. The standard techniques of grinding, polishing., and etching were used in preparing the specimens for metallo-graphic examination. For alloys below 68 pct Cr

Jan 1, 1963

By Carle R. Hayward

(Wilkes-Barre Meeting, June, 1911.) THE growing importance of metallography has caused a corresponding interest in the improvement of apparatus for preparing specimens of metals and alloys for microscopic examination. The purpose of this paper is to describe an electric heating-furnace, a grinding-and-polishing machine, and a device for mounting specimens, which are used in the metallographical work at the Massachusetts Institute of Technology. These three pieces of apparatus were designed and made in the laboratory of the Institute, and. each possesses some original features which may be of interest. ELECTRIC HEATING-FURNACE., The accurate control of heat necessary for metallographic work is best obtained by the electric-resistance furnace. Unfortunately, however, even the platinum-wound furnaces deteriorate with use and ultimately burn out, while the cheaper resistance-materials are often short-lived. Since the resistance-coil must be replaced from time to time, it is of advantage to be able to make this change with as little trouble as possible, and this is an important feature in the furnace shown in Fig. 1. A is a cylindrical galvanized-iron can, with two handles, B. A porcelain tube, C, passes through the central hole in the cover of the can and rests upon the asbestos disk, D; the bottom of the tube is held in place by the asbestos ring, E. The space, F, around the tube is filled with powdered magnesia. G is an ordinary assay-crucible, with the cover inverted so as to present a smooth top for supporting a second porcelain tube, H. The latter is wound with ?Excello " resistance-tape, 0.014

Dec 1, 1911