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By C. D. Tedmon, D. P. Ferriss

THE yield stress, o of low-carbon steel has been shown to vary with the average grain diameter, d, according to the relation1-3 where o is taken to be the lower yield-point stress Of is the friction stress on an unlocked dislocation, and ky is a constant. The interpretation2,4 of ky in terms of dislocation theory relates this constant to the stress to unlock a source across a grain boundary. cottrel14 predicted that ky would increase with decreasing temperature. This was observed to be the case by Adams and coworkers5 in their investigation of niobium (columbium). However, petch6 and Backofen: both working with low-carbon steel, found ky insensitive to temperature. In his work with high-purity niobium, Johnson' found ky equal to zero. Evansg showed that k, was essentially zero for niobium containing nitrogen in an appreciable concentration range. The present experiments were designed to check this apparent anomaly in the value of ky in another Group V metal. Yield points were determined as a function of grain size at several temperatures for tantalum and a tantalum-tungsten alloy. The material used was double are-melted tantalum and a double are-melted alloy of 90 pct Ta and 10 pct tungsten (by weight), both obtained as unannealed, swaged rod. The impurity content of the materials is given in Table I. The tantalum was annealed at 1325"C. in a vacuum resistance furnace using a tantalum boat. The alloy was similarly annealed at 1660°C. Annealing times varied from 15 min to 2 hr, depending on the desired grain size. Nominal pressure in the furnace was 3 X 10~4 mm of Kg. Metallographic examination showed that the annealing treatment produced grain sizes ranging frorn 0.021 to 0.200 mm in the tantalum, and 0.060 to 0.160 mm in the alloy. Tensile bars were made by centerless grinding the annealed specimen;, and then electropolishing to remove all grinding marks. The specimens were than pulled :it 2 1/2 pct per rnin in an Instron testing machine. The tantalum specimens were tested at 77", 195", and 300°K. The alloy was tested at 300°K only. All specimens exhibited a yield-point phenomenon at all temperatures. Typical load-elongation curves at the three test temperatures are shown in Fig. 1. The lower yield stress is plotted as a function of (grain size) in Figs. 2 and 3 for tantalum and the 90 pct Ta-10 pct W alloy, respectfully. The position and slope of the curves was determined by least-

Jan 1, 1962

By Carl F. Cline, Richard R. Vandervoort, Willis L. Barmore

THE objective of this investigation was to determine the high-temperature plastic deformation behavior of stoichiometric uranium mononitride as a function of stress and temperature. Interest in the properties of this material stems from its potential use in high-temperature nuclear reactor systems. The creep of other refractory compounds containing uranium (e.g., U02, UC) has been studied by various investigators.1"4 Fassler et al.4 have studied the creep of UN in vacuum from 1100° to 1350°C at stresses of 6000 and 8000 psi. In the present work, the creep of stoichiometric UN was investigated from 1500° to 1800°C at stresses from 2000 to 5000 psi in a partial pressure of 200 mm of nitrogen. The specimens were prepared by hot isostatic pressing of UN powder into cylinders of $ in. diam by about 1 in. high. After pressing, the specimens were heat-treated in nitrogen at 1900°C for 50 hr. The densities of individual specimens were determined by the water displacement method. All specimens were theoretically dense, based on a value of 14.32 g per cu cm.5 Principal metallic impurities in ppm by weight were: Ca, 50; Cu, 5; Fe, 30; Mg, 5; Ni, 10; and Si, 20. Oxygen content was 400 ± 50 pprn and carbon content was 100 i25 ppm. The nitrogen content was 5.56 ±0.05 wt pct. The average grain size for five specimens, as determined by the intercept method, was 0.14 i 0.01 mm. One specimen had a grain size of 2.0 mm. This large grain size is an anomaly, since all specimens had the same chemical and thermal histories. Specimens of 1/4 in. diam by 1/2 in. high were creep-tested in compression in a clam shell furnace heated by W-25 pct Re sheet elements. Temperature was measured to ilODC by an optical pyrometer which had been calibrated by a standard source. The distance between fiducial marks on the specimen was measured before placement into the furnace. The furnace chamber was evacuated to 10-5 Torr and back-filled to 200 mm N2. After heating rapidly to temperature, the load was applied and controlled to ±2 pct by an Instron testing machine. Upon initial loading, the specimen was deformed until a constant crosshead rate was obtained, then quenched to room temperature, remeasured, and replaced in the furnace. Upon subsequent reloading at temperature, the crosshead rate was constant for the selected condition indicating steady-state creep.

Jan 1, 1969

By A. E. Dwight, A. F. Berndt

ThE published U-Ru equilibrium diagram indicates the existence of six intermetallic compounds in this system.' The structure of only two of the compounds, u2Ru2,3 and URU3,4 have been identified. This communication reports on the crystal structure and density of Uau3, which is formed by a peritectoid transformation at 1025° ± 5°C: U3Ru4 + U3Ru5 = U2Ru3. An alloy with the stoichiometric formula U2Ru3 was prepared by arc melting electrolytic uranium and ruthenium of 99.9 pct purity on a water-cooled copper hearth under an argon atmosphere. After homo-genization at 1000°C for 3 days, a metallographic examination revealed that the peritectoid transformation was complete and less than 5 pct of a second phase was present. A powdered sample, obtained by crushing the brittle compound, was annealed for 1 hr at 1000°C and air-cooled. Debye-Scherrer patterns were obtained with filtered CrKa, FeKa, CoKa, or CuKa radiation. The X-ray patterns of U2Ru3 weFe indexed as an fcc structure with a. = 12.895 0.00lA. The unit-cell constant and its standard deviation were calculated by a computer program described by Mueller, Heaton, and Miller.5 The density, measured by an immersion method, was 14.45 g cm-3. A calculated density of 14.48 g cm-3 was obtained on the assumption that twenty-four formula units (120 atoms) comprise a unit cell. The space group is either oh7 Fd3m, or the less symmetric, T4h, Fd3, since reflections indexed as hk0 with h + k + 4n are absent. All values of h2 + k2 + 12 permitted by both space groups are listed in Table I together with dc, do, and I. values. The calculated d spacings were obtained by the computer program of Mueller, Meyer, and simonsen.6 The observed d spacings above 0.77A were obtained from X-ray" patterns prepared with CuKa radiation, above 0.90A with CoKa radiaaion, above 0.98A with FeKa radiation, and above 1.16A with CrKa radiation. An attempt was made to identify the crystal structure of U2Ru3 by comparison with published data on other A2B3 compounds. A recent compilation7 of intermetallic compounds lists thirty-two structure types with the A2B3 stoichiometry. Only two of the structure types are fcc and they are Sb2O3(r), senarmontite, with 16 Sb2O3 per unit cell, and In2Te3 for which several structures have been proposed.8 However, the two cases cited do not have twenty-four formula units in the unit cell. We therefore, cannot identify UPRU3 with any of the other known A2B3 compounds. Ternary alloys were made in which 5 at. pct Os, Rh, or A1 were substituted for 5 pct of the Ru in U2Ru3. The osmium substitution increased the unit cell constant to 12.899 * .001A, which is to be expected since the atomic volume of osmium is slightly larger than

Jan 1, 1969

By Simon D. Strauss

Production and consumption of nonferrous metals in the United States during 1950 were at peak levels for the postwar period, as is shown in Tables I, II, and III. The trend of production was upward through most of the year. At the year end, with the possible exception of the Tri-State zinc-lead district, the large mining operations in the country were running at capacity. The absence of serious labor interruptions during the year was an important contributing factor in the increased out-put of metals, since in each of the previous postwar years there had been a number of major strikes which affected production adversely.

Jan 2, 1951

By Jeremias K. Chitunda

Significant cost savings and improved ground stability are two initial indications from the current wet process shotcrete ground support program at the Lakeshore mine. The area of shotcrete for ground stability is not strange to the Lakeshore operation. Since the beginning of the project, various shotcrete techniques have constantly been experimented with, incorporating all the latest technological developments. Over the years, the use of shotcrete has been employed as a primary, temporary, or permanent support, singly or in combination with rockbolts and steel sets. The extent of shotcrete usage compared with steel sets and rockbolts has varied from time to time as dictated by the overall state of the art. In 1972, for example, the ratio of the linear drift footage supported with shotcrete to that supported with steel sets averaged 1.0. In 1973, that ratio was about 3.0. Overall, for the Lakeshore mine, there are about 8000 drift ft of shotcrete, 8000 drift ft of steel sets and timber, 750 drift ft of formed concrete, 21,000 drift ft of rockbolts, and 3700 drift ft of combined type support.

Jan 12, 1974

By G. R. Palmer

The occurrence of mercury minerals in precious metal-bearing ores has long been noted. During cyanide leaching of these gold-silver ores, some mercury forms a soluble cyanide complex, which is present in the pregnant leach solution and passes through the process operations of the cyanidation mill. As a result, mercury is found on the electrowinning cell cathodes, on the stripped carbon before It is volatilized during carbon regeneration, or in theme tailings pond. The U.S. Department of the Interior's Bureau of Mines is examining the effectiveness of two ion-exchange resins to adsorb gold and/or mercury from a cyanide leach solution. The resins, Duolite A-7 and Ionac A-305, were contacted with leach solutions containing varying concentrations of mercury, gold, and silver. The resin A-7 reached a maximum mercury loading of 0.0165 lb Hg/ft3, and A-305 reached a maximum mercury capacity of greater than 0.44 lb Hg/ft3. Adsorption of gold by both A-7 and A-305 is influenced by the presence of additional ions in the solution.

Jan 1, 1984

By N. O. Johnson

THE Hog Mountain mine is a pyritic-gold property in the north central part of Tallapoosa County, Alabama, at an elevation of 800 ft. in the southern Appalachian region. It is 13 miles by a good secondary road from Alexander City, a station on the Central of Georgia Railroad. Since its discovery in 1839, the mine has been worked intermittently. The records of past operations are few and are scattered over a long period of time; however, available information indicates a production of approxi-mately 12,000 oz. of gold prior to the present company's activities, which started in 1933. Additional 7844 oz. has been produced under the direc-tion of the present management. The ore from stopes has averaged 0.200 oz. gold per ton; the ore from development, 0.136 oz. gold per ton. Silver, copper, iron and sulphur are also present but to date are of minor importance. The grade of ore in comparatively narrow veins makes necessary extreme vigilance in the methods of mining.

Jan 1, 1937

By J. S. Kirkaldy, R. C. Dorward

The solubilities of copper and gold in silicon and germanium have been determined by equilibration of the solid semiconductors with coexisting liquidus phases. The experimental results were combined with estimated activity coefficients of the liquidus alloys to determine the following partial molar enthalpies and excess entropies of solution for the systems: Solubility measurements were also carried out below the eutectic temperature of the copper-silicon system. The partial molar enthalpy and excess entropy of copper in silicon with respect to Cu3Si were determined to be 40.2 ±0.5 kcal per mole and 9.7 i 0.5 cal per mole — OK, respectively. It has been dentonstrated that nu-cleation and growth of intermediate compounds are retarded in copper-silicon diffusion couples. This points out the dangers of determining equilibrium solubilities by dijjusion methods. THE thermodynamic requirement for equilibrium between contiguous phases at constant pressure and temperature is that the chemical potential of each component be constant throughout the system. Equating expressions for the chemical potential of solute, component 2 say, in two phases, alpha and beta, gives

Jan 1, 1969

By G. W. Reimers, S. E. Khalafalla

A colloidal solution of a ferrimagnetic material, such as magnetite, in a liquid that is immiscible with and lighter than water is projected for use in selective separation of particles according to their density spectrum. Magnetic levitation forces can be created as an antigravity field when the fluid is properly placed in an inhomogeneous magnetic field. When the gradient of the magnetic field is directed downwards, the levitation force in the fluid will be in an upward direction to float sinking nonmagnetic bodies by counterbalancing their density mismatch with the magnetic fluid. Several nonmagnetic objects with densities ranging from 2.50 to 11.35-g cm' were made to float or submerge at will in a 0.96-g cm' density fluid placed in vertical magnetic field gradients ranging from 0.1 to 1 kilo-oersted cm-'. The magnetic levitation force in dyne cm' was found to vary linearly as a function of the object-fluid density mismatch with a slope equal to one g, the acceleration due to gravity.

Jan 1, 1974

By A. S. Malicsi, R. J. Lipp, I. Iwasaki

A loch-grade copper-nickel deposit, with an estimated 4.6 Gt (5 billion st) and average analyses of 0.6% copper, 0.2% nickel, occurs in northeastern Minnesota. In addition to copper, nickel, cobalt, and precious metals, the Duluth gabbro contains magnetite, ilmenite, olivine, plagioclase, and biotite. It u estimated that flotation tailings that would be produced by a concentrator of optimal size to sustain a smelter would amount to 20 Mt/a (22 million stpy). The flotation tailings, having already been ground, warrant a closer examination for recovery and use of potential byproducts. Residual sulfide minerals and fibrous minerals may also be isolated and treated separately for useful purposes or for disposal in an environmentally acceptable manner. Two flowsheets were developed; one involving preconcentration by low- and high-intensity magnetic separation and another involving preconcentration by gravity concentration. Concentration methods for recovering and purifying individual byproduct minerals were investigated. From their chemical, physical, and mineralogical characteristics, the potential areas of application and marketabilities of each product fraction were surveyed.

Jan 1, 1985

By R. O. Scattergood, P. Beardmore, M. B. Bever

THE stored energy and microhardness of a Au-Ag alloy deformed by explosive loading were measured previously as functions of shock pressure' and compared with corresponding data for drawn wires.' The difference of the two processes has been explored further by investigating the annealing behavior of explosively loaded specimens and drawn wires. Sheet specimens, 0.042 in. thick, of a Au-Ag alloy containing 82.6 wt pct Au were explosively loaded in stacks of four.3 Wires prepared from the same melt of alloy were drawn through dies.' The annealing kinetics were determined by microhardness measurements on separate specimens for each annealing temperature and time. Several values of the stored energy were measured by tin-solution calorimetry Experimental details are given elsewhere. Wires were drawn until the microhardness or stored energy equalled the corresponding values of the explosively loaded specimens as nearly as possible. Wire drawn to a true strain 7 of 0.09 had approximately the same hardness and stored energy as specimens explosively loaded to a shock pressure of 70 kbar. The microhardness of specimens

Jan 1, 1963

By R. J. Caro

The Anaconda phosphate plant was put into operation in the fall of 1923. Its present daily operating capacity is approximately 170 tons of treble superphosphate and 16 tons of phosphoric acid analyzing 42 pct P2 O5 and 52 pct P2 Os, respectively. As a result of the continued increased demand for phosphates, Anaconda decided in 1947 to expand the plant's daily output to 270 tons of treble superphosphate and 54 tons of phosphoric acid. The present daily plant intake is 335 tons of wet (footwall) phosphate rock analyzing 31.7 pct P² O5 and 0.28 pct V² O5. The rock is shipped from Anaconda's mine at Conda, Idaho, in open railroad cars, having been crushed to pass 3/8 in. mesh at the mine.' The expansion program will require an increased intake of 300 tons of rock per day. The hanging-wall rock anaIj-ses approximately 30.5 pct P2 O5 and 0.11 pct V² O5, and will be beneficiated in a new washing plant under construction

Jan 1, 1950

(The following list contains the names of those members of the Institute of whose connection with military service we have only recently become acquainted; it also includes the names of a few who have recently been promoted or transferred, indicated by a *. A complete list was published in the Year Book, issued as a supplement of the Bulletin for March, 1918.) *AMBLER, HARRY A., 1st Lieutenant, 0. R. C., 30th Infantry, A. E. F. BAKER, R. F., Private, Intelligence Section, Headquarters 90th Division. *BARTON, L. A., Captain, 604th Engineers. *BATTEN, H. L., Lieutenant, Canadian Engineers, C. E. F. *BENSEL, J. A., Major, U. S. Reserves. BIRKETT, HOWARD, Lieutenant, Aviation, U. S. Signal Corps. BLOOMFIELD, E. C., Lieutenant, 1st Canadian Tunnelling Co. BOOTH, L. E., Watertown Arsenal, Det. E. 0. C., N. A., Watertown, Mass. *BOWMAN, REGINALD G., 1st Lieutenant, Engineers, U. S. R., Int. Ord. Dept. No. 4, A. E. F. *BRADLEY, CLARENCE I., Convois Automobile Section 585,. S. S. U., P. A. R., B. C. M.

Jan 7, 1918

President H. M. Howe, Boston, Mass. (communication to the Secretary): Le Chatelier's pyrometer is certainly a most convenient and accurate instrument for the laboratory, and one that may be used under some conditions in the mill. I have used it for several years and with great satisfaction. Like Prof. Roberts-Austen and unlike Herr Blass, I have always found that its indications remain constant over long periods. Like Prof. Roberts-Austen, also, I find it possible, in a quiet place, to read with extreme accuracy ; and, by the use of a telescope, I can read temperatures to within a degree, for some delicate determinations which I have in hand. Variations in the temperature of the room affect the readings of the instrument far less than one would expect. When the current is cut off, the mirror does not always return exactly to the same place; in other words, the zero shifts appreciably, and must be determined often, indeed every few hours if accuracy be desired. In some cases I have had it determined within a very few minutes of every important reading. To this end a switch should he introduced, so that the circuit may be broken readily. With this arrangement we can determine accurately the position of the zero within a very few seconds of the time of taking any especially important reading. The chief causes of the variation of the zero which I have noticed are as follows: a. The suspension may not be tight enough, so that the momentum of the galvanometer frame as it swings makes its supporting wires slip in their bearings. b. Changes in the position of neighboring iron objects may deflect the mirror. c. Changes in the temperature of the room may, perhaps, change the torsion of the suspension wires, and so shift the mirror. d. Dust may attach itself to the galvanometer frame, and by friction against the surrounding fixed parts of the galvanometer, may

Jan 1, 1895

By K. L. Komarek, P. F. J. Landler

Synthetic polycrystals of wustite were reduced ilz H2-H2O mixtures over limited roncentration ranges wiltun the wustite. field and the weight changes were continuously followed with a McBain quartz spiral balance. The reduction was. found to be controlled by a combined surface plus solid-state diffusion reaction. The solid-state diffusion had an activation energy of 38 kcal. Self--diflusioities of iron decreased with itzcreasing vacancy concentration. The activation energy of. the surface reaction runs different tor- different samples. The surface reaction-rate constan increased with increasirzg vacancy concentration. THE reduction of the oxides of iron has been studied for many years. Edstroem' has summarized the early work and has provided much information on the reduction of magnetite and hematite by hydrogen and carbon monoxide. More recent summaries are those by smeltzer2 and Themelis and Gauvin.3 Most investigators have reported that the iron metal which forms the outer layer during gaseous reduction is rather porous. According to Kohl and Engel14 the formation of such a porous iron layer depends on the properties of the underlying wiistite layer, on the reaction of the gas with the wustite surface, and on the transport of matter through the wustite layer. McKewan, Quets, Wadsworth, and Lewis, and Knacke 10 have found that, if a porous iron layer is formed, a surface reaction between gas and wustite at the bottom of the pores controls the rate of reaction. Seth and ROSS 11 and Warner 12 have pointed out that the influence of the gaseous pore diffusion through the porous iron layer cannot be neglected. It has further been shown that the wiistite layer formed during reduction is dense and that transport of matter across the layer occurs only by solid-state diffusion of iron ions.13,14 The solid-state diffusion rates observed by Edstroem and Bitsianis 14 and the surface reaction rates observed by Quets eta1.' show that an interaction of the two steps in controlling the reaction rate has to be considered. In this investigation the reduction of wustite was studied with respect to the interaction of the two steps, isolated from any other effects, by reducing wustite within the wustite field from higher to lower oxygen concentrations with H2-H2O gas mixtures. A similar study with CO-CO2 mixtures has been performed by Levin and wagner.15 Fused synthetic wustite polycrystals were reduced in steps of 0.4 wt pct from 24.4 to 23.2 wt pct 0 and over a temperature range from 700" to 1050°C. A few tests were also conducted with reduction steps from 24.4 to 23.6 wt pct 0 and 24.5 to 23.2 wtpct0. The Fe-O phase diagram is shown in Fig. 1 where the composition of the gas phase in equilibrium with the condensed phases is plotted as pct H2 vs the temperature. A careful study of the literature led to the conclusion that the fully drawn equicomposition curves (in wt pct O) in the wustite field used by Edstroem 1,16 and other authors needed some correction. Based on results by Darken and Gurry17 (shown as open circles) and on some of our own data, four corrected curves for 23.2, 23.6, 24.0, and 24.4 wt pct O were calculated (drawn as dashed lines in Fig. 1) which should replace the fully drawn equicomposition curves. MATERIALS AND APPARATUS Materials and Specimen Preparation. Wustite was prepared from iron sulfate (Fisher Scientific Co., New York) which had a purity of over 99.92 pct, with small amounts of manganese, copper, and zinc adding up to 0.03 pct. From the aqueous solution iron oxalate was precipitated and decomposed to magnetite according to Economos. 18 The magnetite powder was pressed into cylinders and sintered in vacuum at 900°C for several hours. The sintered compacts were placed in a platinum crucible of 2.5 cm diam which was fitted into a high-purity alumina crucible and then inserted into the center of the graphite heating element of an electric resistance furnace.lg The furnace was evacuated to below 1 p Hg and the magnetite sample was slowly heated. The evolution of gases during heating deter-

Jan 1, 1967

By F. B. Richards

For the last five years the furnace-men drawing their oresupply from the Lake Superior districts have had to solve the problem of using the very fine Mesabi ores as part of their oremixture. It is not my purpope to dwell on the early experiences and the progressive development in the use of these ores up to this time, but to lay before the members of the Institute one prominent feature concerning them, namely, the frequent and sometimes very disastrous slips (?) or explosions (?) occurring at furnaces where these ores are used. The Transactions of the Institute contain very little on this subject. Mr. F. E. Bachman, in his discussion of Mr. 0. 0. Laudig's paper (Trans., xxvi., 1061), advances a theory as to the cause of these occurrences; but this is the only reference to the subject in the Transactions up to this time, so far as I can recall. Probably all the furnace-men running the harddriven coke-furnaces in the central West have had more or less experience with this trouble; and I believe the majority of

Jan 1, 1899

By Hermann Bach, Walther Hänig, Willi Gehrhardt, Ernst Theurich, Walter Langner

With the construction of the Magdeburg zinc works, the Georg von Giesche's Erben Mining Co. of Breslau has to a certain extent completed the program of reconstruction which it set as its goal after the boundaries of Upper Silesia were drawn by the Treaty of Versailles. During its history, covering.more than two centuries, zinc and lead mining has been its chief activity. Through the new boundaries established, it lost to Poland all its mines and smelters, including five distillation smelters. Of its extensive properties, there remained only an apparently unimportant and unexplored portion of the old Bleischarley ore field which, however, happily made possible the resumption of its old business. In 1925 the Deutsch-Bleischarley shaft-only a few kilometers from the old Bleischarley shaft—was sunk and developed, and in May 1926 production of lead and zinc ore was resumed. As facilities for smelting were lacking, the ore was at first delivered to the neighboring smelters, which had now become Polish. Realization of the plan to build its own zinc works had to be postponed at first for lack of capital. In the meantime, however, plans for the new works were worked out in all details. After extensive experimentation in a semicommercial pilot plant it was decided, at the end of 1928 and the beginning of 1929, to use the electrolytic process and, for economic reasons, to place the works at Magdeburg. With zinc at the approximate price level that had ruled since the Deutsch-Bleischarley mine had begun working, it was hoped that the plan could be completed in 1930 with the company's own resources. However, falling metal prices, already noticeable in 1929, made this impossible, and further postponement for a time became necessary. Finally, at the end of July 1933, the funds for building the works became available, in the form of a loan granted under the first employment

Jan 1, 1937

By R. F. Mehl, R. F. Bunshah

A fast amplifier technique has been developed for the measurement of the rate of propagation of martensite in an Fe-29.5 pct Ni alloy. The time of formation of one plate of martensite is 3x10 sec and the rate of propagation is 3300 ft per sec approximately. IT has been known for some time that the plate-like structural unit of martensite forms from austenite with great rapidity. Wiester1 and Hane-mann, Hofmann, and Wiester took motion-pictures of the transformation as it occurs in a 1.65 pct C steel; they demonstrated that a single plate formed fully in the time interval between successive frames, viz., 1/20 sec, thus setting an upper limit. Forster and Scheil,3 using an Fe-Ni alloy with 29 pct Ni, recorded the sonic characteristics of the process electrically, upon an oscillograph, setting the upper time limit at 0.002 sec. Forster and Scheil,~ measuring the change in electrical resistance in the same alloy upon a cardiograph, set a limit of 0.02 sec. Forster and Scheil5 later, employing the same alloy, improved their technique, reporting an upper limit of 7.10 sec. In studying signals of such short duration, it is an important question whether the frequency response of the electrical system used is high enough compared to frequency of the pulse measured, or, put differently, whether the system is able to reproduce without distortion the signal arising, in this case, from the formation of a single martensite plate. Forster and Scheil (referring only to their last paper) obtained signals of a frequency of 30 kilocycles (hereinafter kc); this was about the frequency response of the equipment used; thus, if the signal had a frequency higher than 30 kc, it would still appear as a signal of frequency 30 kc. All of these results thus provided upper limits only. Recent developments in electronics have made available equipment with very high frequency response, very high sweep-speeds, high gain, etc. The electrical characteristics of such equipment, used in the present study, are given in Table I. Such equipment offers obvious attraction in the study of the rate of propagation of a martensite structural unit—and perhaps of other structural alterations proceeding at a very high rate. This paper reports an attempt to develop a technique employing such equipment to measure the time of propagation of a martensite structural unit and the variation of this with temperature, with the mode of formation—athermal and isothermal—in both polycrystalline and single-crystal samples; and from such measurements to obtain the rate of propagation. As will be seen, the results obtained are useful theoretically. Materials All data presented here are for an Fe-Ni alloy of the following analysis: 29.5 pct Ni, 0.027 pct C, 0.135 pct Mn, 0.094 pct Si, balance Fe. There were several reasons for choosing this alloy: 1—it is substantially the one used by previous investigators; 2—it exhibits both the athermala and the isothermal' mode of formation of martensite, both studied in detail by Machlin and Cohen; 3—the subzero temperatures of transformation in this alloy are experimentally very convenient; 4—it exhibits the "burst phenomenon";" 5—the change in electrical resistance upon the formation of martensite, a decrease, is great, approximately 50 pct.' The polycrystalline specimens were in the form of wires of 0.025 in. diameter; the single crystals were 1x1/4x1/4 in. Experimental Methods Electrical Apparatus: Fig. 1 is a schematic drawing of the electrical circuit used. The principle used in these measurements is the same as that used by Forster and Scheil." A small direct current, about 1 to 2 amp, is passed through the sample. When a martensite plate forms, the resistance of the sample changes and a high frequency signal is generated. This signal is picked up by the probes attached to the sample, fed into the bank of amplifiers and thence to the vertical deflection plates of a cathode-ray oscilloscope. The signal itself triggers the oscilloscope trace which flashes across the tube face and is photographed by means of a 35 mm movie camera at the end of a light-tight hood. The camera has no shutter. As soon as the signal flashes

Jan 1, 1954

By A. Yoshikawa, T. Sugeno

To detenmine the origin of the sharp fatigue limit in many ferrous metals, S-N curvces were determined in push-pull fatigue at 18.6 kc per sec at room temperature and - 67°C for various kinds of iron. These differed in carbon and nitrogen content and grain size (25 and 2500 grains per sq mm). Sharp knees appeared in the S-N curves of fine-grained specimens with high interstitial content at both temperatures. In coarse-gruined specimens, knees were not sharp .regardless of the interstitial content and the testing temperature. It is concluded from these results that the controlling factov for the appeavance of the sharp fatigue limit is not strain aging but grain size. It has already been mentioned that iron and some iron alloys show fatigue curves characterized by a more or less sharp knee and a fatigue limit.' Explanations of the origin of this characteristic behavior of fatigue in iron appear to fall into two broad classes. One is concerned with interstitial impurities through the aging or locking effect and the other is based on intrinsic plastic properties of iron. Levy and sinclair2 and Lipsit and Horne3 have suggested that the fatigue limit observed generally in iron and steel is due to interstitial solute aging during the course of fatigue. On the other hand, Thompson and wadsworthl have suggested that the fatigue limit may be analogous to the sharp yield point, in the sense that alternating stresses above the fatigue limit are necessary to break down the dislocation locking. However, there are some experimental results which cast doubt on the general validity of these suppositions.4-8 Ferro and Montalenti' have recently suggested that the typical form of the fatigue curve of iron seems to come from an intrinsic plastic characteristic of the iron structure. This suggestion is based on the experimental result that pure iron containing an insufficient amount of interstitial solute to alldw appreciable strain-aging effects still showed a fatigue limit at room temperature. Although systematic investigations on the effect of grain size are scarce, it is thought that this effect is important in relation to the sharp fatigue limit. In fact, sensible differences were observed by Oates and Wilson4 in fatigue behaviors of a low-carbon steel depending on grain size. Ideally, the fatigue limit will be defined as the upper limit of stress amplitudes at which the life is infinite. This ideal fatigue limit can never be determined because of the limited time available for experiments, and moreover scattered data points often leave the construction of S-N curves somewhat arbitrary. And, it is usually stated that a material has a fatigue limit when its statistical S-N curve becomes apparently parallel to the N axis with a more or less sharp knee. The meaning of the fatigue limit and the sharp knee will be discussed in detail in relation to the construction of S-N curves. The origin of this sharp knee was investigated by determining S-N curves of iron for various interstitial contents, testing temperatures, and grain sizes. EXPERTMENTAL PROCEDURE The material as received was a commercial-grade low-carbon steel in the form of 4-mm-diameter rods with the following composition in weight percent: C, 0.09; Si, 0.017; Mn, 0.43; P, 0.006; S, 0.012; Cu, 0.11. Five different groups of specimens were tested. The grain sizes and interstitial contents in each group are given in Table I. The specimens of group C-02 were decarburized by annealing for 100 hr at 700°C, followed by an additional 100 hr at 850°C in wet hydrogen. Specimens of groups N-2 and N-9 nitrided in a mixed atmosphere of ammonia and hydrogen after an initial treatment identical to group C-02. The specimens of group C-9 were prepared in a manner similar to those of group C-02, except heat treatment was carried out in a vacuum. After polishing their surface with emery paper, the specimens of all groups were given a final anneal for 30 min at 930°C and air-cooled in an evacuated quartz tube. For group C*-9 this

Jan 1, 1965

By D. B. Hunter, H. W. Rosenberg

The titanium-rich portion of the Ti-Pd system was investigated from 0 to 75 wt pct Pd by metallo-graphic and X-ray techniques. A 0 eutectoid occurs at 24 wt pct Pd and 1190°F. Two compoutzds are indicated in the region below 75 wt pct Pd, Ti,Pd and Ti2Pd3. The solubility of palladium its a titanium is low, probably less than 1 pct. In 1960 Rudnitskii and Birunl published a complete version of the Ti-Pd phase diagram. However, their work was in disagreement with the earlier literature in that they reported only one inter metallic compound, whereas three had been reported earlier. In view of these discrepancies, it was therefore necessary to redetermine those portions of the diagram of immediate interest. The following account describes our work on the system over the range of 0 to 75 wt pct Pd. MATERIALS AND METHODS Distilled titanium sponge and elemental palladium were used in the formulation of the alloys; the chemistry of these materials is detailed in Table I. The alloys were prepared as 10 to 50 g blended compacts that were melted into buttons by arc melting under gettered argon on a water-cooled copper hearth. Weighing of the ingredients before and after melting showed that negligible weight changes occurred. Therefore, no analyses were undertaken and the compositions of all alloys are nominal. All alloys were fabricated by hot rolling at 1700°F to 0.070-in.-thick sheet. Scale was removed by sandblasting and pickling in a 5 pct HF-35 pct HNO,, balance H20 solution. For metallographic examination, specimens were mounted after heat treatment transverse to the rolling direction, ground on silicon carbide papers of increasing fineness to 600 grit, and then electro-polished using a solution containing 600 ml me-thanol, 60 ml perchloric acid, 360 ml butyl cello-solve, and 2 ml "Solvent X". Unless otherwise specified, etching of alloys containing up to 42 pct Pd was carried out by swabbing with a 12 pct HN03-1 pct HF aqueous etch where a bright etch was required, or by a 1 pct hydrofluoric in saturated oxalic acid solution where contrast between phases was required. The Ti-52.8 Pd alloy was etched with a solution of 25 ml HF, 40 ml glycerine, 35 ml methanol, and 18 g benzalkonium chloride. For X-ray examination, 1/2-in.-square speci- mens of sheet were mounted flat in a standard 1-in. metallographic mount and ground and polished as above. X-ray diffraction was performed using a Norelco type 12045 Diffractometer, employing CuKa radiation with a nickel filter at 40 kv and 20 ma. Specimens were rotated about the sheet normal during exposure. Although this procedure did not remove the effects of sheet texture from the relative intensities, it had the advantage that oxidation or contaminants entering during preparation of powder samples could not confuse the patterns obtained. RESULTS AND DISCUSSION Fig. 1 illustrates the Ti-Pd phase diagram according to Rudnitskii and Birunl with the work of the present authors superimposed. Both interpretations agree that the system is of the 0 -eutectoid type with an extensive 0-phase field, and that the eutectoid temperature is just below 1200°F. There is also agreement that the solubility of palladium in a titanium is restricted. Our work would indicate that the a solubility of palladium is low, probably less than 1 pct. However, whereas Rudnitskii and Birunl place the eutectoid composition at 41 wt pct Pd, this investigation shows it to be at about 24 wt pct Pd. Moreover, this investigation confirms the existence of compounds at Ti2Pd and Ti2Pd3, whereas Rudnitskii and Birun report only a single Berthol-lide phase covering the TiPd to TiPd, range. Laves et a1.' and Wallbaum, whose work was summarized by Maykuth , reported the existence of Ti2Pd3 and TiPd, in addition to Ti2Pd. More recently, Nevitt and Downe~' have reported the structure of

Jan 1, 1965