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By B. Wilshire, W. J. Evans

W. J. Evans and 8. Wilshire SEVERAL recent investigations1-6 have shown that the strain, c, during transient and steady-state creep is well-represented by the expression: € = e0 + et(l - e-mt) + Esl [l] where Eo is the instantaneous strain on loading, ET the total transient strain, C, the steady creep rate! and m a constant relating to the rate of exhaustion of transient creep. However, it has been noted6 that deviations from this equation occur over the first 10 to 15 pct of the transient stage, when the creep rate, (. decreases more rapidly than is predicted by this equation. This rapid decrease has been attributed to a large change in work-hardening coefficient. It 1s widely accepted that steady-state creep results from a balance between the rate of strain hardcning h and the rate of recovery r (=-s(st) as: dE/dt = Es = r/h [2] Comparison of values obtained for h at the end of the initial extension and during steady creep suggests that h increases several fold during the transient stage. which has the effect of reducing the creep rate proportionally.7 To examine the dependence, on r and h, of the deformation behavior during transient and steady-state creep. a series of constant-stress creep tests was carried out at 413°C at 6000 psi using 70-30 a brass. Prelinlinary investigation showed that. with this material. the transient stage constituted a significant portion of the total creep life (-0.4tf. where tf is the time to fracture). The alloy. obtained from Metals Research Limited. was made from high-purity copper, 99.999 pct. and zinc. 99.99 pct. Heat treatment at 675°C for 4 1/2 gave a uniform grain size of 5 mm-1. Details of specimen preparation and creep testing procedures have been given previously.6 Values of h (?s/?E) were determined by measuring the instantaneous strain. ?E. which occurred on increasing the stress during creep by a small amount. ?s. Similarly. v (= -?s/ ?t) was derived from the incubation period. At, after a small decrease in stress.' Several values of v and h were obtained throughout duplicate creep tests. using different stress increments in the range 300 to 800 psi. The accuracy with which Eq. [I] represents the present creep curves was established by determining the best value of the constants Es, Et, m , and 6, using a digital computer program based essentially on the graphical solution for this equation devised by Conway and Mullikan.9 About 40 strain/time readings were taken during transient and steady-state creep. Over most of the creep curve, the average difference between the measured reading and the calculated strain at the appropriate time was less than 0.0001. However.

Jan 1, 1969

By K. M. Kolobova, E. Z. Kurmayev, A. Z. Menshikov, S. A. Nemnonov, V. A. Trapeznikov

The present work represents a review of our intestigations into the X-ray spectra of solids, which have been carried out by us along two lines of upproach: 1) St@ of the electronic structure of high -rnelting compounds of transition metals; 2) stzddy of the interatomic binding forces by the fine structure of absorption spectra under varying temperature and concentration conditions. With this in mind, int>estigations hare been made into the emission and absorption spectra of the K-series of atoms of transition elements in alloys and compounds. In the problem concerned with the electronic structure of high-melting compounds of transition metals, considerable importance is attached to the question of ascertaining the role played by 3d4sp electrons of metal and 2p electrons of metalloid in the formation of chemical bonds and of giving, on the strength of this data, an explanation of the properties which seem to be contradictory at first sight: good conductivity inherent in metals and high brittleness and high-melting characteristics typical of covalent compounds. Over the last few decades this question has attracted the attention of many investigators whose studies were devoted to this type of compound. Many works, both of theoretical1-3 and experimental4- l5 nature , have contributed much to the elucidation of the physical character of the phenomenon referred to. Alongside the investigations in the field of electric resistance, Hall effect, paramagnetic susceptibility, electronic heat capacity, and the temperature of transformation into a superconducting state, we should particularly emphasize the studies on X-ray spectra, which have played a significant role in the development of the zonal theory for high-melting compounds. This fact has become highly evident after the theoretical calculation of the energy spectrum has been made and the density of states curve in Tic, TiN, and Ti0 has been plotted by Ern and Switendick3 who used the method of augmented plane waves. Correlation of the results of the theoretical calculation of the band structure in the compounds listed above with the data obtained by X-ray spectroscopy studies showed that X-ray spectra can be a source of valuable information on the electronic structure of high-melting compounds within a wide range of ener- gies. It is well known that X-ray emission spectra basically give a direct picture of the occupied excited states above the Fermi level of a solid (valence band, conduction band) and that the absorption spectra (region of initial absorption) give a similar picture of states corresponding to the unoccupied levels near the Fermi surface. Full information on the density distribution of electronic states by energies can be obtained by combining the emission and absorption spectra. Such an opportunity arises from investigation

Jan 1, 1970

By J. G. Morlet, A. R. Troiano, H. H. Johnson

Delayed failure in steel occurs by controlled initiation and growth of a crack. The incubation period for crack initiation was measured. Crack initiation and Propagation are controlled by interaction between hydrogen concentration and triaxial stress state. The incubation period results from stress-induced diffusion of hydrogen to the point of crack initiation. THIS paper describes the phenomenon of delayed failureland the kinetics of crack initiation and propagation in uniformly hydrogenated steel. The investigation was prompted by service failures of high-strength-steel components at applied stresses far below the conventional yield strength, after the part had successfully sustained equal or higher stresses for an extended time interval. This delayed failure phenomenon, often termed static fatigue, is associated1 with the presence of hydrogen. This is not surprising, since the voluminous literature on flaking and hydrogen embrit-tlement demonstrates that hydrogen may exert a potent embrittling influence. Flakes, or internal hairline cracks in alloy-steel forgings, are related to the presence of hydrogen retained from the steel-making process.2 On the other hand, embrit-tlement arises from hydrogen introduced during surface treatments such as acid pickling or electroplating. Laboratory delayed failures have been induced in notch specimens of 4340 steel by electrolytic charging of the specimen surface with hydrogen and subsequent static stressing.l,4,5 Static fatigue was observed over a wide range of applied stresses; however, failure did not occur below a critical applied stress, designated as the static fatigue limit. In this instance the extended time for failure resulted primarily from the macroscopic redistribution of hydrogen. A crack formed to the depth of the hydrogen enriched "case* upon loading; further crack growth naturally awaited diffusion of hydrogen into the material ahead of the crack. The crack-propagation rate was therefore controlled primarily by the macroscopic diffusion of hydrogen into the specimen interior during the test. Thus, in this instance static fatigue was associated with the movement of a gross concentration gradient. However, delayed failure in steel of uniform hydrogen concentration is of greater fundamental interest, as well as commercial significance. With a homogeneous hydrogen distribution a different mode of delayed failure might be expected. As the heterogeneous hydrogen distribution became more uniform,4,5 the initial crack-propagation rate decreased markedly and, in fact, what appeared to be an incubation period for crack initiation was observed. However, the macroscopic concentration gradient precluded an accurate evaluation of these observations. Although the existence of an incubation period, up to this time, has not been established definitely, it is not amiss to point out some implications of the concept. It is of interest in all hydrogen-induced embrittlement phenomena, such as flaking, delayed failure, and hydrogen embrittlement. Much discussion has centered around the possibility of an

Jan 1, 1959

By R. S. French, W. R. Hibbard

FOR tensile deformation, if the stress value is defined by the ratio of the load to the actual area, and the strain value by the natural logarithm of the ratio of the immediate length to the original gauge length of the sample, the resulting data when plotted with logarithmic coordinates result in a linear relation extending from the initial plastic yielding through the maximum load and in some cases, such as for copper and brass, to fracture'.'. The normal form of the curve, therefore, is a parabola, satisfying the following equation: S = Kem [1] where S and e represent true stress and strain, K is a constant, and m is a coefficient evaluating the slope of the curve and designated therefore as the strain hardening coefficient. Hollomon² has reported that this coefficient is a function of the yield strength as effected by grain size in alpha brass, and the carbon content and heat treatment of steel. In the case of steel, the value of the proportionality constant is a function of the carbon content. It was further shown in that paper2 and also by Low and Prater -hat, if the power relation between stress and strain remains valid, the strain hardening coefficient m, is equal to the strain at the maximum or necking load. Thus, an added significant feature is that this coefficient may serve as an index of the capacity for deformation prior to localized necking and subsequent fracture, e.g. drawability. The constant K may be defined as the strength of the material at unit strain. Together the K constant and the m coefficient describe an alloy's physical properties as far as strength and ductility are concerned for a particular yield strength and, in the case of steel, a particular carbon content. The work of Lacy and Gensamer4 gives data on alloy ferrites from which very close estimates of the strength of ternary and higher iron alloys have been made. It was the purpose of this investigation to develop similar data for commercial copper base alpha solid solution alloys. Preparation of Specimens Commercial binary alloys of copper with aluminum, beryllium, cadmium, nickel, silicon, tin and zinc were investigated. In addition, laboratory castings were made of a 1 pct silicon alloy and a 2 pct aluminum alloy to complete these particular series. Two types of copper were used, oxygen free OFHC and tough pitch FC. The analyses of these alloys are shown in table I. Standard ASTM sheet tensile specimens were used to determine the usual physical properties of each alloy and to obtain stress data at strains from 0.0005 to 0.01. Small (1/4 in. x 3 in. x tk.) samples

Jan 1, 1951

By P. M. Robinson, M. B. Beaer

The heat of formation at 0°C of the intermetallic compound AgMg as a function of composition has been determined by tin-solution calorimetry. In this technique, the heat of formation is determined as the difference in the heat effects, at infinite dilution, on dissolution of the compound and a mixture of its components added alternately to liquid tin from a reference temperature, such as 0°C. The experimental technique and method of calculation have been described elsewhere.' The compound AgMg is a 0 electron compound with a CsCl structure.2 In nonstoichiometric compositions of the compound, atoms of the excess component are substituted on the AgMg lattice.3,4 The homogeneity range is approximately 43 to 52 at. pct Mg at room temperature and 38 to 65 at. pct Mg at 500Oc.2 Single-phase alloys outside the homogeneity range at room temperature can be prepared by quenching. The specimens used in this investigation contained from 39.0 to 54.8 at. pct Mg. They were made available, together with analyses, by the Research Laboratory of the General Electric Co. Metallographic examination of the quenched specimens containing 39.0 and 54.8 at. pct Mg gave no indication of the presence of a precipitated phase. The measured heats of formation are listed in Table I. In a calorimetric run, four to six additions each of a specimen and the corresponding mixture of the components were made. One or two calorimetric runs were carried out with each composition depending on the amount of samples available. The limits stated in the table represent the experimental precision and not the absolute accuracy of the measurements. Thermodynamic investigations of the compound AgMg have been made by Trzebiatowski and Terpilowski 5 and Kachi.6,7 The heats of formation at 500°C derived from the combined electromotive-force values of these investigators8 are more exothermic than the heats of formation at 0°C reported here, Fig. 1. The differences cannot be explained by the difference in temperature. This is shown by the published heat capacity of the stoichiometric compound, which obeys the Kopp-Neumann rule from 0" to 500oC.9 The heats of formation derived from equilibrium data are generally considered to be less accurate than those determined by calorimetric methods because small errors in the change of the equilibrium values with temperature have a large effect on the calculated value of the heat of formation. The heats of formation derived from the combined published electromotive-force values reach a maximum at 56.0 at. pct Mg.8 Kachi reports a maximum of -4.7 kcal per g-atom at the stoichiometric composition.7 The present results also indicate a maximum at or near the stoichio metric composition, Fig. 1.

Jan 1, 1964

By J. H. Westbrook

IT is always of interest to document the origin of real microstructures which closely approach various idealized morphologies. Such instances constitute excellent bases for experimental studies of the effect of microstructure on properties. Typical examples include the eutectoid steels (lamellae) used by many investigators and the two phase Cu-Cr alloys (spheres) recently employed by Hibbard and Hart The present note describes a structure with cylindrical particles. In a study of certain alloys in the Cr-C system, an alloy was arc melted whose composition was very close to the aCr-Cr,C, eutectic (3.2 wt pct C, according to the latest phase diagram published by Bloom and Grant2). The alloy was not analyzed but previous experience with the melting technique employed indicates good correspondence between intended and analyzed compositions with negligible tungsten contamination from the electrode. The phases present in the alloy were identified by X-ray powder patterns as a chromium and Cr,C,. Typical micrographs, presented in Fig. 1, show unmistakable evidence of the cylindrical geometry of the carbide phase. The eutectic grains are randomly oriented and, consequently, only a few show the true fibrous nature of the carbide particles, most being cut so as to show slightly elliptical cross sections. Within any particular grain, remarkable uniformity is to be observed with respect to the size, shape, spacing, and orientation of the carbide particles. Length to diameter ratios have been estimated from the micrographs to be at least 250:1, with diameters of about lp. This alloy may be of further interest from different viewpoints. On the one hand, it might be used to check the applicability of the equations derived by Fullman3 for computing true particle dimensions of cylindrical particles from opaque random sections. On the other hand, it might be possible to extract the carbide particles from this alloy and repack them in a ductile matrix to form a synthetic structure of the type discussed by Metcalfe et al.4 With the large l:d ratio and the small diameter of the carbide fibers, it is likely that the interdefect distance in each fiber is sufficiently great to permit realization of a large fraction of the presumed high strength of the carbide. References 1W. R. Hibbard, Jr. and E. W. Hart: Dispersion Hardening of Copper-Chromium Alloys. AIME Trans., 1955, vol. 203, p. 200; Joun-nal of Metals, January 1955. 2D. S. Bloom and N. J. Grant: The System Chromium-Carbon. AIME Trans.. 1950. vol. 188. p. 41; JouRnal of Metals, January 1950. aR. L. Fullman: Measurement of Approximately Cylindrical Particles in Ooaaue Samples. AIME Trans.. 1953, vol. 197, p. 1267; Journal of Metals. ~ebtember 1953 4 A. G. Metcalfe, C. H. Sump, and W. C. Troy: Fiber Metallurgy. Metal Progress, 1955, vol. 67, p. 81.

Jan 1, 1958

By John L. Lamont, Walter Crafts

STUDIES of the effect of composition of steel on hardenability by Grossmann,1 and as-quenched hardness by Field2 and by the authors,3 have made it possible to predict the results of quenching when the composition and cooling rate are known. In order to extend the application of the hardenability calculation to the quenched and tempered condition in which steel is finally used, a survey has been made of the hardness changes caused by tempering. From this study a method has been developed for the prediction of hardness and tensile strength of steel in the tempered condition. The method of calculation was developed from Rockwell C hardness tests on quenched and tempered Jominy specimens and is expressed in Rockwell C hardness units. It is of an additive type in which the degree of softening from as-quenched hardness is estimated. Tempered properties may be calculated within about plus or minus 5 Rockwell C hardness or plus or minus 15,000 lb. per sq. in. tensile strength. This degree of accuracy is less than that necessary for the control of heat-treatment, but is adequate for the comparative evaluation and selection of alloy steels. The formula indicates that tempered hardness is primarily dependent on as- quenched hardness and, as in the hardening reaction, the progress of tempering is controlled mainly by the carbon content- Alloys tend to retard softening by a secondary hardening mechanism in which the alloy appears to migrate from ferrite to the carbide phase. The factors for the effects of alloys in tempering vary so much from the effects of alloys in hardening that different steels of equivalent hardenability may, after lie heat-treatment, differ considerably in tensile strength. PROCEDURE In developing the method for calculating tempered Rockwell C hardness, simple and complex steels were tested over a range from 0.08-to 0.65 per cent carbon and up to 2.68 per cent manganese, 2.18 silicon, 3.50 chromium, 4.94 nickel, and 1.06 molybdenum. The steels were made as small induction-furnace heats at the Union Carbide and Carbon Research Laboratories, Inc. The accuracy of the method was finally checked on a variety of carbon, low-alloy and high- alloy types of heat-treating steels produced under commercial conditions. The method was based on a study of tempered Jominy bars, and its validity was tested by correlation with the center hardness and tensile strength of oil-quenched and tempered bars from ¼ to 4 in. in diameter. The method of calculation was derived from the differences in Rockwell C hardness between as-quenched and quenched and tempered Jominy specimens. Prenormalized Jominy hardenability specimens quenched from a normal temperature for austenitization were used to obtain a range of as-quenched Rockwell C

Jan 1, 1946

By Walter W. Bradley

(Three, papers included, in this discussion are classified as Mining Geology and also as one of the following-A, Metal Mining: B, Milling and Concentration: L, Geophysics. These papers are TP 2255, TP 2092 and TP 2038.) CONTENTS [PAGE Review of Fluorescence as Applied to Minerals, with Special Reference to Scheelite. (TP 1967 by J. W. VANDERWILT, Min. Tech., March 1946. Discussion by WALTER W. BRADLEY) I Geologic Interpretation of Magnetic Exploration on the Mesabi Range, Minnesota. (TP 2038 by R. B. H. JONES, Min. Tech., July 1946. Discussion by ROBERT B. SOSMAN) I A Technique for Photographing Difficult Subjects through a Petrographic Microscope. (TP 2092 by DONALD W. SCOTT, Min. Tech., Nov. 1946. Discussion by HORACE WINCHELL) 2 The Search for Concealed Deposits-a Reorientation of Philosophy. (TP 2146 by SAMUEL G. LASKY, Min. Tech., May 1947. Discussion by T. M. BRODERICK)3 Occurrence of Lead-zinc Ore at Iron King Mine, Prescott, Arizona. (TP 21 go by H. F. MILLS, Min. Tech., July 1947. Discussion by HUGH M. ROBERTS)3 Geologic Relations and New Ore Bodies of the Republic District, Washington. (TP 2197 by LAWRENCE B. WRIGHT, Min. Tech., July 1947. Discussion by AUGUSTUS LOCKE and J. A. RICHARDSON) 4 San Manuel Prospect. (TP 2255 by H. J. STEELE and G. R. RUBLY, Min. Tech., Sept. 1947. Discussion by L. KENNETH WILSON, ELDRED D. WILSON and the author) 5] Review of Fluorescence as Applied to Minerals, with Special Reference to Scheelite WALTER W. BRADLEY*-AS I recall, the first portable units for ultra-violet light of practical use with scheelite were developed at the Nevada-Massachusetts Tungsten Mine at Mill City, Nevada, and were used underground. Ultra-violet lamps are also installed there in the mill, above the gravity-concentration tables, for control observations. Geologic Interpretation of Magnetic Exploration on the Mesabi Range, Minnesota ROBERT B. SOSMAN*-When artificial precipitated magnetite is oxidized at a temperature in the vicinity of 100°C, the oxide is converted into a chocolate brown ferric oxide of the formula Fe2O3, free from ferrous iron, yet possessing the same magnetic susceptibility as the original Fe3O4. This form of Fe2O3 is variously called "ferromagnetic ferric oxide," " maghemite," or "gamma ferric oxide," and has been found as a natural mineral. If a body of magnetite in the Biwabik were to oxidize to this form, the oxidized and leached ore body might successfully conceal itself from Mr. Jones' survey by this ferromagnetic pretense. So far, gamma ferric oxide has not been found on the Minnesota iron ranges. I thought I had found some in the Hibbing pit in 1940, in a strongly magnetic specimen of soft ore differing in color from the prevailing hematite

Jan 1, 1947

By J. W. Hickman, E. A. Gulbransen

In a previous paper' the authors have investigated the structure of the oxide films formed on most of the metals that make up the alloys of this study. The metals were studied in order to provide basic information on the structures, both physical and chemical, of the oxide films and to determine how these structures are effected by the temperature, time of oxidation, and surface preparation. It was felt that an understanding of the physical and chemical structure as well as the stability of the oxide film might furnish clues as to the nature of the reaction process and the protective quality of the film. The oxidation of the metals was studied over the temperature range 300' to 7o0°C. except for copper, wherc the range selected was 100' to 500°C. The results of these studies were presented in graphical form as existence diagrams of the oxides on a time-temperature scale. For some of the metals the existence diagrams were simple and showed few chemical transitions, but there were numerous cases where the physical state of the oxide surface was a function of time and temperature. In general the physical state of the oxide surface changed with increasing temperature so as to increase the sharpness of the diffraction patterns and to cause orientation effects to be more pronounced. Deviatiois in lattice Darameters from X-ray values were noted. In general these deviations were of positive nature and may be due to solid solution of the metal in the oxide lattice. This effect might be expected in thin oxide films. In a study of the oxidation of alloys containing two or more metals, there may arise the complicating factor of identification of the oxides formed. A thorough understanding of the oxides formed on the pure metals, therefore, was, essential before investigation of the oxidation of alloys. In this paper it is our purpose to present a study of the following problems: 1. The existence diagrams of various alloys. 2. The effect of the structure of the alloying metal on the existence diagram of iron. 3. The effect of the percentage of chromium on the oxides formed on Fe-Cr alloys. 4. The relationships, if any, between the oxides formed and the protective quality of the oxides. The following alloys are included in this study: alloys of iron with body-centered cubic, face-centered cubic and other metals, 13 Cr-Fe, 18-8 stainless steel, K4²B, Nichrome V, Hipernik, Inconel, Stellite "²I," Refractaloy, Kovar, mild steel, a series of Cr-Fe alloys and a series of Co-Fe alloys. Since many of the commercial alloys in this list contain more than two metals, various complicating factors in the identification of the oxides formed may arise.

Jan 1, 1947

By E. A. Gulbransen, J. W. Hickman

In a previous paper' the authors have investigated the structure of the oxide films formed on most of the metals that make up the alloys of this study. The metals were studied in order to provide basic information on the structures, both physical and chemical, of the oxide films and to determine how these structures are effected by the temperature, time of oxidation, and surface preparation. It was felt that an understanding of the physical and chemical structure as well as the stability of the oxide film might furnish clues as to the nature of the reaction process and the protective quality of the film. The oxidation of the metals was studied over the temperature range 300' to 7o0°C. except for copper, wherc the range selected was 100' to 500°C. The results of these studies were presented in graphical form as existence diagrams of the oxides on a time-temperature scale. For some of the metals the existence diagrams were simple and showed few chemical transitions, but there were numerous cases where the physical state of the oxide surface was a function of time and temperature. In general the physical state of the oxide surface changed with increasing temperature so as to increase the sharpness of the diffraction patterns and to cause orientation effects to be more pronounced. Deviatiois in lattice Darameters from X-ray values were noted. In general these deviations were of positive nature and may be due to solid solution of the metal in the oxide lattice. This effect might be expected in thin oxide films. In a study of the oxidation of alloys containing two or more metals, there may arise the complicating factor of identification of the oxides formed. A thorough understanding of the oxides formed on the pure metals, therefore, was, essential before investigation of the oxidation of alloys. In this paper it is our purpose to present a study of the following problems: 1. The existence diagrams of various alloys. 2. The effect of the structure of the alloying metal on the existence diagram of iron. 3. The effect of the percentage of chromium on the oxides formed on Fe-Cr alloys. 4. The relationships, if any, between the oxides formed and the protective quality of the oxides. The following alloys are included in this study: alloys of iron with body-centered cubic, face-centered cubic and other metals, 13 Cr-Fe, 18-8 stainless steel, K4²B, Nichrome V, Hipernik, Inconel, Stellite "²I," Refractaloy, Kovar, mild steel, a series of Cr-Fe alloys and a series of Co-Fe alloys. Since many of the commercial alloys in this list contain more than two metals, various complicating factors in the identification of the oxides formed may arise.

Jan 1, 1947

By T. E. Leontis, D. H. Feisel

MAGNESIUM alloys containing rare earth metals have received considerable attention during the past several years because of the need for light alloys having high strength and creep resistance at elevated temperatures. Although much of the work reported earlier has dealt with alloys containing Mischmetal, it has been shown in two previous papersl, V hat distinctly different effects are produced by various rare earth metals and rare earth metal mixtures on the properties of magnesium. For example, much higher strengths are obtained in magnesium alloys containing didym-ium (essentially neodymium plus praseodymium) than in alloys made with Mischmetal, which contains all the rare earth metals in the proportions in which they occur naturally in the monazite ore. Mg-rare earth metal alloys are characterized by a relatively coarse grain size, which greatly impairs castability. The addition of zirconium as a second alloying ingredient has been shown8,7 to refine the grain size, which also produces a distinct improvement in the strength properties. Certain Mg-Mischmetal-Zr and Mg-Mischmetal-Zn-Zr alloy compositions which are currently being produced commercially have been discussed in dytail by Nelson and Strieter,8,4 who also present some in- formation on a Mg-low Ce-Mischmetal-Zr alloy, and by Nelson.8 A patent issued to Jessup, Emley, and Fisher9 emphasizes the superiority of Mg-didymium-Zn-Zr alloys over the corresponding alloys made with Mischmetal. The purpose of this paper is to present the results of an extensive investigation concerned with the effect of increasing amounts of zirconium on magnesium sand casting alloys containing several different rare earth metal mixtures in varying amounts. The effect of the addition of zinc to some of these alloys is also being reported. Preparation and Testing of Alloys The alloys studied in this investigation were prepared in small laboratory melts according to the melting procedures described by Nelson1" as the Crucible Method. Electrolytic magnesium having the composition shown in Table I was used as the starting material. The rare earth metal alloying ingredients used in preparing these alloys were essentially of the compositions listed in Table 11. Some of the didymium-containing alloys were prepared using a Mg-didymium hardener. The rare earth metal content of this hardener analyzed 1.2 pct Ce, 10.4 pct Pr, 80.8 pct Nd, and 7.6 pct La. The zirconium was added in one of three forms: 1) as sponge zirconium obtained from the Bureau of Mines; 2) as a fused salt consisting of 50 pct ZrCl, and 50 pct alkali chlorides from which the zirconium is reduced by the magnesium; or 3) as a Mg-Zr hardener. The alloying procedures and melt hand-

Jan 1, 1958

By N. K. Chen, R. Maddin, K. T. Aust

Lattice rotations occurring on the tension and compression sides during the bending of molybdenum single crystals at room temperature were followed in detail. Observations were also made concerning crystallite rotations and slip traces. &apos;The results indicated the participation of (110) as slip planes and the<111>as slip directions. Crystallite fragmentation during bending was also noted. EVERAL investigations have been conducted on pure bending of face-centered cubic metals.&apos;-" Structural changes as a result of "bend-gliding," and the importance of bending and constraints during conditions of axial stressing, have been noted.&apos;," It was evident that the mechanism by which the bending deformation occurs is more complex than the case of simple shear. Studies of the bending of body-centered cubic metals from the aspect of the crystallographic mechanism appear to be lacking. Molybdenum single crystals therefore were subjected to deformation by bending in order to determine the reaction of the body-centered cubic lattice to bending stresses. It might be expected for the bending of single crystals that lattice rotation as represented by the axis of compression would proceed toward the pole of the active slip plane and that rotation of the tensile stress axis should indicate the slip direction.&apos; It was believed therefore that a study of the tension and compression sides of bent molybdenum single crystals should give data concerning the operative slip system. Specific problems which are pertinent to the overall picture of plastic deformation were also investigated, e.g., whether the constraints offered by pure bending give rise to the deformation band, and also the nature of the asterism occurring on the tension and compression sides during the stages of deformation. Experimental Procedure Eight single crystal specimens were grown from sintered molybdenum rods 143 in. diameter using the method described previously.6 The purity of this material was reported as 99.9 pct as described elsewhere.&apos; The specimens were % to 1/10 in. in diameter x 7 in. long, with single crystals approximately 1 to 2 in. in length occupying the entire center sections of each specimen. The specimens were elec-trolytically polished using an electrolyte of 300 cc methyl alcohol, 60 cc H2SO4, 130 cc HCl, and a current density of 4 amp per sq in. Each specimen was then loaded in a bending apparatus similar to that used by Yen and Hibbard,&apos; as shown in Fig. 1. The load was applied by means of a spring and screw arrangement through four ball-bearing surfaces set 1.5 in. apart. Either the inner two bearings or the outer two (A, B, Fig. 1) were attached to a movable steel plate (D) through which the load was transmitted. Since the apparatus was mounted on a track of the X-ray apparatus, the tension or compression side of the specimen could

Jan 1, 1954

By J. Gordon Parr, G. R. Purdy

The phase boundaries of "TiNi" have been accurately determined by high-tewperature X-ray diffraction and metallo-graphic techniques. The phase (centered at 51 pct Ni) has a restricted range of homogeneity at 500°C, and a much greater range at 800°C. "TiNi" in all alloys containing less than 51 pct Ni decomposes rapidly and reversibly at 36°C to form a previously unreported phase. ThE region of the titanium nickel system corresponding to the phase "TiNi" has been the subject of several investigations.1,2,4-7 Laves and wallbaum1 reported "TiNi" as a body-centered cubic (a2) Phase, and Duwez and Taylor2 determined its para- meter to be 2.986. Duwez and Taylor also reported that "TiNi" decomposed into "Ti2Ni" and "TiNi3" on prolonged heating at 650" and 800°C, which led McQuillan3 to suggest a sluggish eutectoid reaction between "TiNis" and "Ti2Ni". Margolin, Ence, and Nielsen,&apos; working with higher purity alloys, found no evidence of this decomposition. They showed the "TiNi" phase region extending from 49 to 54 pct*

Jan 1, 1962

By J. R. Cahoon, W. V. Youdelis

FOR the diffusion of copper in silver-rich alloys, there have been only two previous investigations, that of Seith and Peretti in 1936, and that of Sawatzky and Jaumot2 in 1957. Seith and Peretti obtained a value of 24.8 keal per g-atom for the activation energy of diffusion whereas Sawatzky and Jaumot obtained a value of 46.1 keal per g-atom. Admittedly, Seith and Peretti used relatively high concentrations of 2 at. pet Cu and polycrystalline diffusion couples, while Sawatzky and Jaumot investigated tracer diffusion in single crystals of silver. The difference in the results, however, seems too large to attribute solely to solute concentration, as a change of over 20 keal per g-atom in the activation energy suggests a change in the mechanism of diffusion. Therefore, in the present investigation the diffusion coefficient for copper in polycrystalline Ag-2 at, pet Cu alloy is re-established using conventional sandwich-type diffusion couples and electron-probe microanalyses, and the results are compared with those of the previous studies. The diffusion couples were prepared from high-purity silver (99.999 pet) and high-purity copper (99.999 pet). The silver disks, 1/4 in. long and 4 in. in diam, were machined from an ingot which had been solidified in a dynamic vacuum of 10-3 mm of Hg to eliminate oxygen absorption which otherwise would result in copper oxide precipitation in the weld zone. The alloy disks of similar dimensions were machined from an alloy ingot (nominal composition 2 at. pet Cu) which had been unidirectionally solidified to obtain a predictable solute concentration,3 and homogenized for 1 week at 800°C. Sandwich diffusion couples were made by pressure welding an alloy disk between two silver disks in an induction heating coil. The couples were diffusion-annealed at temperatures of 800°, 756°, 699°, and 630°C in tube furnaces in which the temperature was controlled to better than ± l°C. The diffusion couples were examined metallographically for weld defects, and couples showing even minute defects at the weld interfaces were rejected. Concentration penetration curves were established using an A.R.L. Microprobe analyzer. CuKO radiation was counted and converted to concentration using 0.5 and 1.0 wt pet Cu chemically analyzed standards. Initially, four continuous profiles were obtained, and averaged to obtain the final diffusion curve. The initial analysis was performed commercially and the welds were not located with respect to the profile. Therefore, the results were rechecked by the authors using the Mellon Institute A.R.L. probe. In the latter case, concentrations were obtained at 10-µ steps for four different traverses, and then averaged to obtain

Jan 1, 1968

By H. J. Levinstein, W. H. Robinson

A method of chemically polishing silver for metal-lographic examination has been developed. The samples are prepared by polishing on 0, 2/0, and 3/0 paper. They are then polished on 600 micro-cut paper, followed by a final mechanical polish on a cloth containing 5µ diamond paste. The samples are then chemically polished in a solution of 100 cc of saturated chromic acid and 5 cc of a 5 pct HC1 solution. The chemical polishing is performed by swabbing with a cotton ball saturated with the solution. During the chemical polishing, the sample is rinsed frequently in running water. Polishing in this manner for 5 min is sufficient to remove the strained material from the previous polishing operations. The amount of material removed is approximately 4µ/min. The surface obtained is flat and free of pits. Fig. 1 is an interference micrograph of a silver surface polished by this technique. If the solution employed is of improper HC1 content, an interference color film will form on the sample. This film can be removed either by swabbing with a cotton ball saturated with ortho-

Jan 1, 1962

By J. F. Nicholas

THE angles between the crystallographic planes in cubic metals were originally given by Bozorth and have been republished many times. Recently, Salkovitz2 tabulated the angles for the hexagonal metals (magnesium, zinc, and cadmium). he most commonly used metal which does not fail into either of these groups is tin, which has a tetragonal structure with an axial ratio of c/a = 0.54558 (99.99 pct purity, 25°C).² ccordingly, Table I has been prepared giving the possible values for the angle, 4, between planes of the types {HKL) and {hkl). The formula used was: Hh + Kk + LI — cos? = —--------------—-----------— A [(H2 + K2 + L2-a2c2(h2 + k2 + r;)] All angles are given correct to the nearest minute as this is sufficient for all practical purposes. Every angle depends in a different way on variations in the value of c/a, but even in the worst cases a variation of about 0.0003 in this ratio is needed to vary an angle by l&apos;, which corresponds to a temperature change of 20 °C or can be caused by impurities.

Jan 1, 1952

By Horace W. Hindry

This paper presents the ingredients composing a type of oil-base mud that has been successfully used in drilling oil horizons in California, the effect of ingredient concentrations on physical properties, methods of handling at the well and possible advantages of a waterless drilling fluid with excellent plastering properties. INTRODUCTION AN oil-base mud is a rotary drilling fluid in which oil has been substituted for water as the principal liquid ingredient. In recent years such a mud has been developed and used successfully for drilling the oil horizons of wells in various California fields. There are several types of oil-base mud, but only the type that is currently used to any appreciable extent will be considered at this time. The oil-base drilling-mud compositions used by Shell Oil Company, Incorporated have been covered by several patent applications on which patents are expected to issue at an early date. The purpose of this paper is to present data on the fundamental design of the mud; the ingredients used and their specifications; the effect of ingredient concentration on physical properties; the selection of the proper mud; the facilities needed for handling the mud; and a general discussion [oil] drilling with oil-base mud. In view of the early stage of development of oil-base mud, the great number of variables, and the almost unlimited possible combinations of these variables, which in turn require extensive laboratory study, there are certain irregularities and omissions in the data presented here. However, it is believed that sufficient data are at hand to permit a fairly complete analysis of the characteristics of oil-base muds. In view of the excellent plastering properties of oil-base mud when properly proportioned, its use should: (I) minimize the possibility of impairing the natural flow potentialities of the producing horizon such as that resulting from infiltration of water from water-base muds; (2) permit smaller clearances for setting liners, since the mud sheath has no appreciable thickness; (3) eliminate the possibility of clogging the perforations of the liner with thick mud sheath; (4) facilitate the removal of the mud sheath from the walls of the hole, for its mud sheath has no appreciable strength; (5) assist in drilling through formations, such as "heaving shale," where water wetting appears to be a source of difficulty. (6) permit cores to be obtained without contamination from drilling water. FUNDAMENTAL DESIGN OF AN OIL-BASE MUD In the design of any rotary drilling mud it is necessary to select materials that will fulfill the following requirements: (I) act as the liquid medium and regulate the viscosity; (2) impart initial and final plastering properties; (3) give gel strength and structure in order to prevent settling; (4) serve as a weighting material. The

Jan 1, 1941

By L. D. Jaffe, H. C. Mann, E. L. Reed

The authors have recently published1 evidence that brittle transgranular fracture of polycrystalline metals does not originate at a point and propagate continuously across the material, but rather develops at numerous related points, leading to a series of micro-cracks which subsequently link up. Series of related microcracks were observed in steel specimens broken in fatigue—specifically, at the central portions which broke during the final sudden fracture. Microcracks of the type mentioned have also been reported by Baeyertz, Craig and Bumps&apos;2 in steel broken under impact. % Some micrographs published by Irwin3 may possibly be interpreted as showing discontinuous brittle cracks. This paper presents additional observations of the authors on discontinuous crack propagation under various conditions. Impact Test Specimens The impact test specimens were cut longitudinally from a steel forging containing: The heat treatment consisted of oil quenching in a heavy section from 1600°F and tempering at 1260°F. The resulting yield strength was 78,000 psi, tensile strength 100,000 psi, elongation 20.0 pet in 2 in., and reduction of area 55.0 pet. Standard V-notch Charpy specimens were broken in a 217 ft-lb machine at a striking velocity of 16.8 fps. Energy absorption and fracture appearance of this material in the V-notch Charpy test are plotted as functions of temperature in Fig 1. After test, fractured halves of specimens appearing 0, 40, 80, and 100 pet fibrous (to the unaided eye) were electroplated with nickel, sectioned longitudinally (perpendicular to the notch at its midpoint), polished and etched with Cohen-Hurlich-Jacobson (C-H-J) reagent (picric acid plus Zephiran chloride in ethyl ether)4 or with Vilella reagent (1 pet picric plus 5 pct hydrochloric acid in ethyl alcohol).5 Fig 2 and 3 show cracks near the path of final fracture in the specimen rated 0 pct fibrous. Many of the cracks terminate at the boundaries of ferrite grains, some at boundaries of pre- existing austenite gzains. * A crack often starts near the end of another. Cracks within the same ferrite grains are parallel or approximately parallel in several cases. A large percentage of the cracks are branched. Fig 4 illustrated a group of cracks in the 40 pct fibrous specimen. Branching and parallelism are well marked. No more than three directions of crack have been observed on the polished surface in one ferrite grain. This is consistent with the evidence6 that brittle fracture of ferrite takes place on the cube face crystallographic planes: the {100} planes. The appearance of some cracks suggests that they have passed around a projecting corner of a second ferrite grain by going outside the plane of polish. In Fig 5 cracks in the 80 pet fibrous specimen may be observed. Some of

Jan 1, 1950

By H. J. Modi, P. L. De Bruyn

IN recent years interest has been aroused in flotation rate studies both from a technical and a more practical aspect. With increasing fineness of grind becoming a necessity in treatment of low grade ores, difference:; in flotation rates of various size ranges will assume importance in the evaluation of overall recovery results. Theoretical analysis of flotation kinetics was initiated by Schuhmann,&apos; who sought to define flotation rate of a given mineral and specified size range in terms of certain physical variables of the flotation system. Using as a basis for his analysis the bubble-particle encounter hypothesis previously advanced by Gaudin,&apos; Schuhmann writes for the rate of flotation (R,.) of particles of average size x, Rx = PcPa(x) V F. [1] In this relation Pc and Pa represent, respectively, the probability of collision between particle and gas bubble in a given time interval and the probability of adhesion of particle to the bubble after collision. Rigorously speaking, the term PC does not have the significance of a probability factor, since it depends on the time interval and therefore can be numerically greater than unity. The term c(x) expresses the concentration of particles of an average size x in the flotation cell in weight per unit volume of pulp, and V denotes the total volume of pulp in the cell. The product, P,c(x)V, defines the frequency of particle-bubble collisl.on, and when it is multiplied by P,, the number of collisions per unit time resulting in successful adherence is obtained. The factor, F, measures the froth stability and is introduced because after fruitful bubble-particle contact some particles may still riot reach the froth launder. Coalescence of bubbles in the froth column or too short a bubble life could account for this effect. Schuhmann also introduced the concept of "specific flotation rate" (Q) to allow for the relative abundance of different mineral species in the flotation pulp. The specific flotation rate, having the dimension of reciprocal time, is defined as Eq. 2: Qx =Rx/c(x)v [2] and it also follows from Eq. 1 that Qx = PcPaF. [31 The theoretical aspects of flotation kinetics were also considered by Sutherland,3 who tried to improve Eq. 1 by expressing the probability factors in terms of such physical variables as particle radius (x), bubble radius (X), velocity of bubble relative to particle (v), the number of bubbles per unit volume of pulp (N) and the induction period (A) necessary for air-mineral adhesion. According to Sutherland&apos;s treatment, the rate equation, Eq. 1, transforms to R, = [3pX x v N] [sech2 (3 v ?/4 X) ] ?c(x) V [4] where the first term in brackets on the right-hand

Jan 1, 1957

By G. E. Tardiff, A. A. Hendrickson

THE objectives of this communication are to present the solid-solution strengthening data for silver-base zinc single crystals and to evaluate the importance of strength contributions from several mechanisms through the use of this data combined with that for the silver-base aluminum case.&apos; Some features of the yield point behavior of silver-base zinc crystals were previously reported.&apos; Silver-base zinc alloys were prepared by induction melting 99.99 pct Ag with 99.9 pct Zn in high-purity graphite crucibles contained in argon-filled quartz tubes. After the first melting, the ingots were cut into short lengths, redistributed in the molds, and remelted in order to reduce solute-concentration variations. Alloy single crystals were then grown from the melt through the use of a modified Bridgeman technique which consisted of lowering the graphite crystal mold through a hot zone at a rate of 3/8 in. per hr. As in the melting operation, the molds were contained in argon-filled quartz tubes. Gage lengths 2 cm in length were introduced by both spark machining (circular cross sections) and abrading and acid etching (rectangular cross section) followed by electropolishing (a comparison of the critical resolved shear-stress values prepared by the two techniques showed no differences in strength values). The final cross-sectional areas of the crystals were approximately 5 sq mm. Prior to testing, the crystals were annealed at 600°C for 20 hr in argon atmospheres, furnace-cooled, and lightly electropolished. Crystal orientations were determined using the back-reflection method. The tensile testing was done on a Model FM Instron at a strain rate of 1(T4 per sec. Test temperatures of 77", 200°, and 400°K were attained by immersing the specimens in liquid nitrogen, dry ice-acetone mixtures, and silicone oil, respectively. The critical resolved shear-stress (CRSS) values for silver-base zinc crystals as a function of composition and testing temperature are given in Fig. 1. It will be noted that the CRSS for silver-base zinc solid solutions, as in the silver-base aluminum1 case, depends on temperature in a manner typical of fcc solid solutions: at high temperatures (-300°K and above), the CRSS is relatively temperature-independent but becomes strongly dependent on temperature at lower testing temperatures. A reasonable picture of solid-solution strengthening for silver-rich solutions at room temperature based on "direct" strengthening mechanisms3 is as follows. Since silver alloys have low stacking-fault energies, extended dislocations are expected and it is possible that Suzuki locking4 makes the major contribution to the room-temperature solute strengthening. This provides essentially temperature-independent strengthening since thermal motions of the dislocation line are not large enough to aid the dislocation in escaping the solute atmosphere extending over the fault width. An estimate of the

Jan 1, 1964