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By M. V. Lowry

This paper outlines the economic considerations that led to the recent installation of a thickener at St. Joseph LeadCo.'s Balmat, N.Y. mill. To incorporate storage of concentrates, they decided upon a single, unusually deep tank to be used for both storage and thickening. The abnormally high rake lift required was achieved by the novel feature of having the entire drive platform raise and lower. Initial operating problems are described along with the satisfactory solutions. Total costs for concentrate handling before and after installation of the storage thickeners are compared. In Northern New York State, the St. Joseph Lead Co. conducts a 2100 tpd zinc mining and milling operation at its Balmat Plant. Conventional crushing, grinding, and flotation is used to produce a zinc concentrate. For 32 years, from 1930 through 1962, the plant operated with the concentrates going directly from flotation to the filtering, drying, and loading facilities. All of the concentrate handling equipment, therefore, had to operate 24 hrs per day. It also had to accommodate wide fluctuations in tonnage, due to variations in the grade of ore. Many problems were thereby encountered in filtering and drying, but it was never concluded that the cost could be justified for installing a conventional, large diameter thickener. Finally, in 1963, they installed an unconventional thickener that is unusual in several respects. The tank depth is 16 ft instead of the normal 8 ft. The rakes are raised and lowered by having the main drive gear located on a movable platform. Automatic controls are programmed to raise the drive platform and rakes during one shift of storage. During the next two shifts of withdrawal, the controls are programmed to lower the drive platform and rakes. After three years of operating this unique storage-thickener, the conclusion is that a correct choice was made from several alternative schemes for storing concentrates. The various considerations involved in the final selection will here be analyzed, and the design features and installation details will be de- scribed. Operating problems and modifications made to the equipment will next be considered, and finally the effects upon filtering, drying, and loading will be reported. SELECTION CONSIDERATIONS Even without a thickener, concentrate handling had become reasonably efficient at the Balmat Mill by the year 1962. A tonnage that varied between 6 and 25 tph was being handled fairly satisfactorily. The filter cake moisture of 8%% seemed quite respectable, except that two large filters were usually in service. Three filters often had to be operated in order to prevent excessive filter overflow with consequent loss of values. This situation occurred when zinc concentrates from flotation exceeded 20 tph and when filter cloth blinding developed. Over the years, numerous small improvements had been effected, such as: selection of a filter cloth with better flow characteristics; addition of flocculant to the filter feed; and, in 1953, the smallest of three drum filters was replaced by a five disc, 8' 10" diam filter with a bottom agitator and snap blow. As another example of fairly efficient operation, the oil-fired dryer was doing a seemingly satisfactory job of further reducing the moisture content to an average of 3%. However, there were often considerable dust losses when the tonnage suddenly dropped off to 6 tph. At high tonnage rates, the resulting high moistures of 4% and 5% caused difficulties due to concentrates sticking and freezing in chutes leading to the box car loaders. (Drying of concentrates is justified because of the high freight rate for the long shipping distance to the company owned smelter at Josephtown, Pa. near Pittsburgh.) It was long realized that installation of a thickener would permit the subsequent steps of concentrate handling to proceed more smoothly and would alleviate the problems existing in the filtering, drying, and loading operations. It was also realized that even a slightly lower filter cake moisture could mean considerable savings in fuel oil. However, all these factors were never quite sufficient to warrant the expense of a thickener until three more considerations were added to the picture. First, the advent of flocculants meant that a thickener of relatively small area could now be considered. Secondly, a complete renovation of the zinc flotation circuit was made between 1957 and 1961. The

Jan 1, 1967

By H. I. Aaronson, H. A. Domian, G. M. Pound

The thernodyna,nics of I the Proeutectoid ferrite re-action ha1.e been investigated on the bases of three diifevent descviptions of the statistical thernzodynamics of interstitzal solid solutions. Especially at low ternperatures, substantial dijeretzces are found in the valltes of the extrapolated y/y + a and cr/a + y equilibriurn curls, and in the To- co7nposilion metastable eqliilibriunz curl-es thus co,npited. Although neither actiztity nor phase-diagram date are able to distingrish udeqiutely among the various descviptions, the statustics of Lacher, Fouller, and Guggenheinz provide the ?nost conplete epresentation az3ailable of the single carbon-ctrbon interaction energy (w) nzodel of an intevstitiril solid solution, and the relationships deduced frojrl then2 are accordingly pre.ferred. The findings tlzut w in austenite 'aries significu?ztly uith tenpevntrue and that phase-diagawr data arc not accurately con?palible usith eqcrctions deduced on the basis of actility infoation indicate, hou'e13er, that a wzore cornplex nlodel of the uustenite , und pvobably of the .feyrite, solirl solutions will have to forn the basis of f4tuve statistical t1.eat1nents. Some suggestions for such a ruodel arc advanced. Althoug11 w represents a vepltlsio energy in austozite, it was found to corvcsporzd in ferrite to a binding energy, in qualitatit.e accord zc,itlz the internal-friclion results of Keefer and wert. ThE transformation of austenite to proeutectoid fer-rite is becoming recognized as an exceptionally useful vehicle for quantitative studies of the kinetics of phase transformations.'" Reasons for this popularity include well-characterized microstructures which develop on a convenient scale with acceptable kinetics within a considerable temperature-composition region, the absence of great sensitivity to common impurities, and, especially. the availability of a unique wealth of the ancillary information indispensable for the quantitative interpretation of kinetic measurements, including phase diagram,3 crystallographies diffusivity,5 inter-facial energy,=17 elastiit," specific vlume, ''' and ativity'-' data. Development of considerable amounts of additional thermodynamic information from activity data is of particular importance with respect to kinetic studies, since much of this information is needed in temperature-composition regions not directly accessible to presently available techniques for the measurement of equilibrium properties. A generally useful approach to the thermodynamics of solid solutions, which is of especial value in this situation, is based upon the formulation of the free energy of such solutions as a function of temperature and composition. The free energy of solid solutions has been resolved into many components. Particularly in the case of interstitial solutions, with which we shall be concerned in the present study, however, only the positional entropy component has been intensively studied. The other components are conventionally taken into account by fitting equations for the activity of the interstitial species or the temperature-composition path of phase boundaries, derived principally from positional entropy considerations, to experimental information on these quantities through adjustment of one or more constants in the equations. A number of studies of the thermodynamics of interstitial solid solutions have been made primarily on this basis,'"25 but only Kaufman, Radcliffe, and cohenZ2 (hereafter KRC) and ener''% ave applied the results of such studies to develop relationships for the thermodynamic quantities of interest in the austenite —- proeutectoid ferrite transformation. KRC made use of a model developed by cheil'' (on the basis of a previous study by ohansson'), and subsequently rede-rived correctly by Speiser and retnak,' in which a carbon atom is considered to inhibit occupancy of a certain number of its nearest-neighboring interstitial sites. schei120 determined the number of sites in austenite thus excluded by matching calculated and experimentally measured curves for the variation of carbon activity with the mole fraction of carbon. zener17 used a different approach. He assumed that the positional entropy of carbon is ideal both in austenite and in ferrite (i.e., no excluded interstitial sites), and included all other contributions of carbon in a temperature-independent "free-energy change" accompanying the transfer of 1 mole of carbon between the two phases. This quantity was determined by "pinning" an equation derived for the boundaries of the a + y region to experimental data on the compositions of these boundaries at a single temperature. In the present investigation, three different approaches to the thermodynamics of the proeutectoid ferrite reaction are examined comparatively: I) the method of Zener; 2) the model employed by KRC and predecessors; and 3) the more detailed statistical thermodynamic treatment of the same model developed by acher and Fowler and uenheim, ' in which the problem of overlapping regions of influence of individual interstitial atoms is resolved. In order to make these comparisons, it is necessary to undertake an extension of one aspect of Zener's method; since the Lacher- Fowler -Guggenheim (LFG) treatment has not been previously used in the present context, the necessary thermodynamic "superstructure" for this treatment will be developed in parallel

Jan 1, 1967

By R. E. Mussler, F. E. Block, T. T. Campbell

An exploratovy study was made to deternzine the feasibility of preparing beryllium by the metallother-. mic reduction of beryllium oxide. The procedure involved heating a relatively nonvolatile metal reductant in contact with beryllium oxide in a vacuum. Beryllium vapors formed in the reaction were condensed as a coherent deposit on a heated surface. Reductants tested included tanthanun, yttrium, thorium, Th-Mg, and Zr- Ti alloys, and the hydrides of lanthaniir~z, yttriunz, and zirconiur?7,. Test ten7pevatures ranged from 1350'to 175O' C, and reaction times ranged frot 30 to 100 lzr. In most cases metal recoveries were lola, although yields close to 90 pct of theoretical were obtained with latzthanum, yttrium, and zirconium reductants. In most cases metal deposits were contanzinated by beryllides, /ls/cally of the Beln M or Bel3 M type. BERYLLIUM has a variety of unique properties including light weight (sp gr 1.85), low thermal neutron absorption cross section, high scattering cross section, excellent dimensional stability, high strength to weight ratio, high melting point (1285"C), high specific heat, and high thermal conductivity. Interest in beryllium as a structural material in aerospace and nuclear-reactor applications is based on these properties. In general, the potential of beryllium has been only partially realized, largely because of the brittleness of poly crystalline forms of beryllium, difficulties associated in its fabrication, and joining problems encountered in its use in structural applications. Several excellent books and monographs are available to those interested in the occurrence, extractive metallurgy, and utilization of beryllium.1"* Although an extensive amount of research on beryllium has been in progress during the past 10 years, much of the work has been concerned either with the so-called "ductility problem" or with the development of methods of fabrication and evaluation of properties of various commercial or purified grades of metal. A recent survey of the literature indicates that only limited efforts are presently being directed toward developing new methods for reducing beryllium compounds to metal. Two major commercial methods now used to produce beryllium are the magnesium reduction of beryllium fluoride and e lec trow inn ing of beryllium from fused sodium chloride-beryllium chloride salt baths. Only a limited amount of work has been done on the direct reduction of beryllium oxide. Major factors which complicate this method are the great stability of beryllium oxide and the reactive nature of beryllium metal. The stability of the oxide necessitates extremely high reduction temperatures and vacuum operation to liberate beryllium metal vapor and cause reactions of the following type to proceed: XBeO(s) +YM(s)-MYOX(s) + XBe(& As early as 1939, roll' used this reaction for the direct reduction of beryllia by zirconium and titanium, and later in 1952 ~a~el~ studied the reduction of beryl-

Jan 1, 1967

By P. G. Winchell, R. J. Russell

The distribution of displacements of originally plane surfaces by an invariant-plane strain has been analyzed statistically. The displacement ratio (the magnitude of the displacement of a point originally a unit distance from the invariant plane) can be determined from an analysis either of tilts of random surfaces or of displacements of random scratches scribed on a randowz surface. In either case the mean of the tangent of the observed displacement angle is related to the displacement ratio, and the number of observations used in determining the mean is related to the confidence limits placed on the estimate of the displacement ratio. In estimating the effect of applied stress on a phase transformation whose displacement effects can be approximated as an invariant-plane strain,* the dis- placement ratio of the invariant-plane strain is of primary importance. Two procedures for determining such displacement ratios are considered here. In the tilt method the measured quantity is taken to be the angle through which a random polish plane is rotated by the invariant-plane strain. In the scratch method the measured quantity is taken to be the angle between the original direction of a random scratch in a random polish plane and the projection of its final direction in the polish plane. In order to obtain precise results from either of the methods, it is necessary to measure the relative volume change associated with the strain in a separate experiment. TILT METHOD A locally homogeneous invariant-plane strain, P, with displacement ratio, S, may be written&apos; where ; and < are unit vectors indicating the displacement direction and invariant-plane normal, respectively, as pictured in Fig. 1. Eq. [I] describes a uniaxial strain if the direction of displacement is parallel to the invariant-plane normal and a pure shear strain if the displacement direction is perpendicular to the invariant-plane normal. The original orientation of the random polish plane relative to the invariant plane and to the displacement direction is shown in Fig. 2. The angle 03 between < and u is related to the relative volume change, ?V/V, and to the displacement ratio by As a result of the invariant-plane strain, the polish plane is rotated about its intersection with the invariant plane by the angle y, which is always taken to be positive. The tangent of this angle in terms of the above parameters is

Jan 1, 1967

By P. K. Leung, S. R. Allada, P. M. Dranchuk, D. Quon

The alternating direction explicit procedure (ADEP) makes use of the boundary conditions to reduce multi-dimensional problems to a series of one-dimensional problems. The method, previously applied to reservoirs containing only an under-saturated oil, has now been extended to cover the case of natural gas reservoirs. l his involves solving a non-linear partial differential equation, application of the procedure is straightforward and no calcuIational problems were encountered. INTRODUCTION There has been a growing interest in formulating mathematical models of petroleum and natural gas reservoirs — models which permit the engineer to examine and evaluate the physical and economic consequences of various alternative production policies. The tremendous reduction in the cost of solving such models in recent years has made possible their use as an almost routine management tool. This reduction is the result not only of improved computer hardware but also of the development of more efficient mathematical techniques. The present paper is concerned with the application of a recently proposed numerical method (ADEP) to two-dimensional gas reservoirs. STATEMENT OF THE PROBLEM Given a two-dimensional Region R, bounded by a closed Curve C (Fig. 1) such that the behavior on Curve C is known, the differential mass balance for each fluid phase in R, neglecting gravitational effects and assuming Darcy&apos;s law for fluid transport, can be written as:

Jan 1, 1967

By R. C. Ku, A. J. McEvily, T. L. Johnston

The microplastic response of a series ofas-quenched Fe-Ni-C martensites has been measured at 77°K. At strains less than JO&apos;3 the flow stress is governed primarily by the transformation-induced dislocation structure of the martensite. Only at strains in excess of 10-3 is the influence of carbon manifested in the flow stress. At these macroscopic strains, typically 10-2, the solid-solution hardening is proportional to (wt pct C)1/3, and, in an alloy containing 0.39 wt pct C, amounts to 50 pct of the flow stress. THE technological significance of high-strength ferrous martensite has stimulated many investigations of its structure and properties. Although our knowledge of the characteristics of martensite has increased immensely, especially with the advent of high-resolution techniques, an understanding of the basic strengthening mechanism still remains elusive. The purpose of the present paper is to consider certain aspects of micro-plastic behavior of Fe-Ni-C martensite which we feel can help to resolve this important problem. Such alloys are particularly suitable for experimental investigation because their compositions can be adjusted to reduce the M, to a temperature low enough essentially to eliminate the diffusion of carbon in the freshly formed martensite.1 The mechanical properties in this condition are of interest inasmuch as they reflect a state that is free of the important but complicating influence of precipitation processes. In this virgin martensite the carbon is distributed as it was inherited from the parent austenite; i.e., it is present interstitially, and gives rise to tetragonality through strain-induced ordering.&apos; In order to determine the source of strength of such alloys, Winchell and Cohen1 investigated the low-temperature macroscopic stress-strain behavior of a series of virgin martensites of increasing carbon content but of common M, temperature (-35°C). They found that the flow stress increased rapidly with carbon content up to 0.4 wt pct; beyond this point the flow stress increased at a much slower rate. It was concluded that martensite is inherently strong. To account quantitatively for the strength of virgin or as- quenched martensite in terms of the role of carbon, Winchell and cohen3 suggested that the carbon atoms, trapped in their original positions by the diffusionless martensite transformation, interfere with dislocation motion according to a model akin to that of Mott and Nabarro. 4 In this treatment, individual carbon atoms are considered to constitute centers of elastic strain and thereby generate an average stress resisting the motion of dislocations throughout the lattice. The additional stress necessary to move dislocations, over and above that necessary for motion in a carbon-free martensite, is given by where L is an effective length of dislocation capable of motion. L was assumed to be limited to the spacing between the twins that are an essential structural element of Fe-Ni-C martensites. They assumtd the spacing to be invariant and of the order of 100A. However, recent work5 has shown that L is variable and can be in excess of 1000Å, so that the assignment of an appropriate value of L is not straightforward. In contrast to the above conclusion that there is an intrinsically high resistance to plastic flow, it has been suggested by Polakowski6 that freshly quenched martensite is in fact "soft" in the sense that dislocations are initially free to move upon application of stress. The high indentation hardness and macroscopic yield stress of ferrous martensites are then a consequence of rapid strain hardening that depends upon carbon in solution. Consistent with this point of view are the results of Beau lieu and Dubé who measured the rate of recovery of internal friction as a function of aging (tempering) temperature in a freshly quenched steel containing 0.90 wt pct C, 0.37 wt pct Mn, 0.1 wt pct Cr, and 0.07 wt pct Ni. The kinetics were clearly consistent with the idea that many dislocations are unpinned in the as-quenched state and that during aging they become progressively pinned by carbon at a rate controlled by carbon diffusion in the body-centered martensite lattice. In order to provide a basis upon which to distinguish between the "hard" and "soft" interpretations indicated above, we have made studies of the initial stages of plastic deformation in Fe-Ni-C martensites similar to those&apos;used by Winchell and Cohen. It will be shown that the results support the contention that dislocation segments in as-quenched material are indeed

Jan 1, 1967

By Thomas C. Wilder

The activities of both components and the partial and integral molar thermodynamic properties of mixing for the liquid Al-Ge system at 1200°K and for the gertnanium-rich Al-Ge liquidus have been determined from data for eighteen alloys of compositions in the range 0.0593 < 0.880 using the reuersible gal-vanic. cell in the temperature interval 9320 to 1258°K. The liqui-dus compositions above 93 2 °K loere also ve determined by observing the discontinuities in the C us T plots for the high-melting alloys. This system shows moderate negative deviation from ideality throughout, the values for y° being 0.212 and 0.189 for aluminum and germanium, respectively, at 1200°K. Pavtial molar Properties of aluminum on the germanium-rich solidus and at infinite dilution in Ge(s) oboue 932°K were estimated from the foregozng measurements and the equlibrium data of previous investzgators. RECENT compilations of data1" have shown an increasing demand for knowledge of the thermodynamic properties of mixing of metallic alloy systems. In the case of binary-liquid systems where one of the components is a semiconductor this information is useful because, primarily, properties of the second (dopant) component on the liquidus, solidus, and at infinite dilution may be determined more accurately than from calculations based on the phase diagram. In this investigation a reversible galvanic cell was used to determine the chemical potential of aluminum in the two-phase region, liquid + [Ge], on the germanium-rich side of the A1-Ge system in the temperature range 932" to 1193°K. In addition, similar measurements for homogeneous liquid A1-Ge alloys for the entire composition range were obtained for the temperature interval 932" to 1258°K. The cell used was: The experimental technique and the treatment of the data were essentially the same as described earlier394 and are elaborated upon only briefly here. Each cell consisted of a liquid aluminum anode and three A1-Ge alloy cathodes of different composition which were held in Morganite alumina crucibles. The alloys were made up from aluminum and germanium weighed to the nearest 0.1 mg to a total weight of 5 to 10 g. Aluminum was a gift of Aluminum Co. of America and had a purity of 99.995+ pct. Germanium of transistor grade was a gift of Bell Telephone Laboratories. The four electrodes were contained in a larger alumina crucible which also held the prepurified fused chloride electrolyte. Contact to the electrodes was made by tantalum wire leads sheathed in alumina. The tantalum leads were centered in the electrodes by suitable positioning of an alumina radiation shield which fitted on the top of the - alulnina crucible. Two chrome l-alumel thermocouples, sheathed in quartz wells, completed the internal cell arrangement. The entire assembly was enclosed in an alumina tube, fitted with a water-cooled copper head so the system could be evacuated and then flushed with purified argon. *

Jan 1, 1967

By E. H. Rennhack

When cast hypoeutectic Zn-Ti alloys are rolled, the TiZn15 compound particles arising from eutectic decomposition form a network of fibers promoting improved creep resistance.&apos; The effect is magnified with increasing titanium content and extends to hy-pereutectic concentrations. Strip produced from the latter-type alloys, however, also contains large, primary crystals of the compound that tend to initiate cracking during subsequent fabrication operations. In a study of the influence of various casting modifications on the size and distribution of these crystals, the phase relationships existing between the eutectic and the TiZnIs intermetallic compound in the Zn-Ti system were of major interest. Although several in- vestigators1 4 have explored the equilibria within this compositional range, their results show considerable lack of agreement. Consequently, with the exception of the solvus boundary, the constitution of this system containing up to approximately 1.0 wt pct Ti was . The findings are reported in the present note.

Jan 1, 1967

By S. Shapiro, G. Krauss

RECENT investigations1 3 of the products of marten-sitic transformation in Fe-Ni and Fe-Ni-C alloys have made use of light microscopy to describe mar-tensitic fine structure. The application of conventional metallographic techniques to this problem was possible because of the similarity of distributions of parallel striations developed by etching polished surfaces to distributions of transformation twins which are positively identified in thin films by transmission electron microscopy. The surface striations frequently are not well-defined, and could also be due to, for example, rows of etch pits which are not resolved by the light microscope. This note describes the etching effects revealed by examination of surface replicas of mar-tensite in the electron microscope. The application of a replica technique both extends the observations of fine structure made with the light microscope and allows the results of conventional metallography to be used with more confidence. Samples of an Fe-33 wt pct Ni alloy were used for this study because of the detailed knowledge of the fine structure of martensite which has been developed&apos;-4 for alloys of about this composition. Samples transformed to martensite at -120°C, and transformed samples heated to 340°C to effect a small amount of reversal of martensite to austenite, were examined. Surfaces were first prepared for replication by elec-tropolishing in a chromium oxide-acetic acid electrolyte at a current density of 0.1 amp per sq cm and a temperature of 15°C or a perchloric acid-acetic acid electrolyte at a current density of approximately 2 amps per sq cm and a temperature of 15°C. The polished surfaces were then etched for 4 to 7 sec by immersion in a solution of equal parts HC1, HNO,, and H20. Application of the etchant for this period of time produced discrete attack of certain features without loss of resolution due to overlapping of areas most susceptible to etching. The etched surfaces were replicated by 1) preshadowing with Pt-Pd alloy at an angle of 20 to 30 deg, 2) depositing a thin carbon film, and 3) stripping the film and shadowing material by immersion in a 5 pct nital solution. Two types of etching effects were observed by examination of the surface replicas in the electron microscope: l) continuous striations centered at the bottom of long grooves or the tops of pyramidal elevations on the sample surface, and 2) high densities of fine etch pits. Examples of both types of features are shown in Figs. 1 to 4. The striations are in each case continuous and have the same characteristic configurations as do transformation twins in martensite. Fig. 1 shows that the density of grooves decreases toward the edge of a martensite plate and Fig. 2 shows a region where the striations are of varying length. Similar examples of transformation twin arrangements determined by transmission electron microscopy of thinned foils of martensite have been shown in the literature,&apos;~ and, based on these similarities, the striations and their associated grooves or mounds are considered to be evidence for the presence of transformation twins. The transf~rmation twins in martensite are on the order of l00 A thick, much too fine for resolution by the light microscope. It appears that orientation-dependent etching of the matrix martensite about the twins results in grooves or surface elevations which

Jan 1, 1967

By M. L. Rudee, R. A. Huggins

Samples of iron containing nitrogen or carbon have been given treatments similar to those used in cold-work peak (CWP) measurements and examined by transmission electron microscopy. It was observed that the unusual and nonreproducible behavior of the carbon CWP can be explained by a strong tendency for carbon to form grain boundary precipitates at temperatures below those used for CWP measurements. These precipitates dissolved at the temperatures used in the CWP measurements. There was no evidence for nitrogen precipitation at grain boundaries. There was no indication of precipitation along dislocations in either carburized or nitrided samples given treatments similar to those of CWP measurements. Although it is possible that subelectron-microscopic clustering had occurred, this observation supports the theories of the CWP that are based on continuous atmospheres rather than on individual precipitates. In an earlier paper,&apos; the present authors developed a new distribution function to predict the occupation of sites for interstitial impurity atoms around a dislocation. When this distribution was applied to the case of carbon and nitrogen in iron, it predicted that, if the temperature dependence of the concentration of solute atoms in the matrix was controlled by the presence of equilibrium carbide or nitride precipitates, the tendency for nitrogen to segregate to dislocations would be greater than that for carbon even though their binding energies to dislocations are identical. The cold-work internal-friction peak (CWP) is considered by most authors to be produced by the interaction of interstitial impurities with dislocations. Many investigators have studied the CWP in iron containing carbon and nitrogen and have observed a significant difference between its behavior in the two cases. In this paper a series of experiments will be reported that were initiated to determine whether the application of the new distribution function would explain the observed differences between the carbon and nitrogen CWP. Although it was found that the distribution function, pev se, did not explain the differences, the differences became clear, and some insight into the mechanism of the CWP was realized. Before reporting the present experiments, the literature pertaining to the differences between the carbon and nitrogen CWP in iron and the various mechanisms proposed for the CWP will be reviewed. LITERATURE REVIEW Snoek2 first observed the CWP in iron specimens containing nitrogen, but also reported a weak and unreliable peak in carburized samples. Later, Ke3 established that the CWP height was proportional to the degree of deformation. The presence of nitrogen alone would produce a peak of the same size as found in a sample containing both nitrogen and carbon, and KG concluded that the CWP was caused by nitrogen. In a discussion of G&apos;s paper it was reported that Dijkstra had investigated the CWP in samples that contained only carbon. He found it to be much smaller than the nitrogen peak and "unstable". KG et al.4 charged specimens of iron with both carbon and nitrogen. They observed that the carbon CWP was much smaller than that observed in nitrided samples, but that aging at 300°C caused the carbon peak to increase. A similar treatment produced no change in a nitrogen peak. Annealing at higher temperatures caused the height of the CWP in both the nitrogen and carbon samples to decrease. This behavior was also observed by Kamber et al. 5 who found that the activation energy for the annealing of the CWP was identical with the activation energy for the self-diffusion of iron. They concluded that the annihilation of dislocations by climb caused the reduction in the CWP height. Kamber et al. studied the "unstable" carbon peak in detail. They measured both the Snoek and CWP during various aging treatments. In carburized samples, aging at 100°C caused the Snoek peak to disappear, although the CWP peak remained small. However, a subsequent treatment for 5 hr at 240°C caused the CWP to reach a maximum. They proposed that an additional location for the carbon, other than whatever site produced the CWP, is present. In nitrided samples the CWP was completely developed as soon as a measurement was made; additional sites are not present. No explanation of either the additional site or the difference in the behavior of carbon and nitrogen was offered. petarra5 performed a systematic study of the effect of composition on the CWP. Using three kinds of "pure" iron, he showed that there was a residual CWP when the carbon and nitrogen concentrations had been reduced to less than that detectable by Snoek-peak measurements. He observed the same general annealing behavior and composition dependence as previous investigators, with the following exceptions. On first measuring the carbon CWP, it was found to be identical with the residual peak, and essentially independent of the carbon content. If the CWP was measured a second time in the same sample, it increased in size, but was still only about one-fourth the size of a CWP in a sample of the same iron nitrided to the same composition. On the other hand, a series of annealing experiments showed that the nitrogen CWP was not al-

Jan 1, 1967

By H. J. Morel-Seytoux

The influence of patten, geometry on assisted oil recovery for a particular dispIacement mechanism is the object of investigation in this paper. The displacement is assumed to be of unit mobility ratio and piston-like. Fluids are assumed incompressible and gravity and capillary effects are neglected. With these assumptions it is possible to calculate by analytical methods the quantities of interest to the reservoir engineer for a great variety of patterns. Specifically, this paper presents (1) very brieily, the methods and mathematical derivations required to obtain the results of engineering concern, and (2) typical results in the dorm of graphs or formulae that can be used readily without prior study of the methods. Results of this work provide checks for solutions obtained from programmed numerical techniques. They also reveal the effect of pattern geometry and, even though the assumptions of piston- like displacement and of unit mobility ratio are restrictive, they can nevertheless be used for rather crude but quick, cheap estimates. ,These estimates can be refined to account for non-unit mobility ratio and two-phase flow by correlating analytical results in the case M = 1 and the numerical results for non-piston, non-unit mobility ratio displacements. In an earlier paper1 it was also shown that from the knowledge of closed form solutions for unit mobility ratio, quantities called "scale factors" could be readily calculated, increasing considerably the flexibility of the numerical techniques. Many new closed farm solutions are given in this paper. INTRODUCTION BACKGROUND Pattern geometry is a major factor in making water-fIood recovery predictions. For this reason many numerical schemes have been devised to predict oil recovery in either regular patterns or arbitrary configurations. The numerical solutions, based on the method of finite difference approximation, are subject to errors often difficult to evaluate. An estimate of the error is possible by comparison with exact solutions. To provide a variety of checks on numerical solutions, a thorough study of the unit mobility ratio displacement process was undertaken. To calculate quantities of interest to the reservoir engineer (oil recovery, sweep efficiency, etc.), it is necessary to first know the pressure distribution in the pattern. Then analytical procedures are used to calculate, in order of increasing difficulty: injectivity, breakthrough areal sweep efficiency, normalized oil recovery and water-oil ratio as a function of normalized PV injected.

Jan 1, 1967

By Richard L. Ashbrook, John F. Wallace

Several high-temperature eutectics of cobalt and nickel alloys were modified by small additions of selected elements. Thes-e alloys were compared to unmodified melts for microstructural variations. A few modified compositions were selected on the basis of structure and their tensile and stress-rupture behavior determined. The results of stress-rupture tests in air at 1800 F and room-temperature tensile tests of four high-temperature eutectics showed modification capable of producing substantial improvements in properties. The microstructures were altered and mechanical properties improved by: a.) dispersing a subordinate phase more uniformly throughout the matrix; b) replacing large continuous -network or platelike constituents with small equiaxed discontinuous phases; and c) by forming new, finely divided phases. tHE term "modification" is most commonly used to describe the refinement in microstructure of the Al-Si eutectic that occurs as a result of rapid cooling from the melt or on slow cooling after treatment with small amounts of sodium.1 "Modification" has also been used to describe the change from flake to spheroidal graphite in the austenite-graphite eutectic of cast iron.2 This change of graphite shape is accomplished by small additions of cerium or magnesium.3 Other systems have also been shown to be capable of modification, for example: Pb-Sn by copper;4 Al-Cu by sodium;5 Al-Mn by sodium;5 and Pb-Sb by aluminum.5 Although modification of Al-Si alloys and cast irons is usually accompanied by improved mechanical properties, a general definition of modification has been suggested to include the effect of small quantities of impurity elements on the microstructures of all eutectic alloys, regardless of the effect on the mechanical properties.6 In this paper, the term "modification" is employed in a broad sense to include the formation of third phases or even the supplanting of one of the binary eutectic phases by a third phase. The mechanism of modification, as for any solidification phenomenon, must be considered primarily in terms of nucleation and growth. Although both nuclea-tion and growth mechanisms are required to explain all the phenomena observed in connection with the solidification of modified eutectics, various investigators have usually favored one or the other.7"16 It has been shown that modification of a binary eutectic can be effected by addition of a solute element that has greatly different distribution coefficients or k values in the two phases of the eutectic. Under these conditions, differences in the temperatures at the solid-liquid interfaces of the two phases retard the growth of one phase with respect to the other.4 It has also been shown that increased undercooling favors a transition from a rodlike eutectic to a globular eutectic.17 A mechanism proposed for the transition from lamellar to rodlike eutectics depends on the concept of constitutional super cooling.18 The modification of eutectic alloys may be of interest for high-temperature service as well as at room temperature. Although "high-temperature eutectic alloys" may appear to be a contradiction in terms, many eutectic systems, including those studied in this work, have melting points in excess of 2400°F. One of the mechanisms by which high-temperature alloys are strengthened is dispersion of a relatively brittle phase such as an oxide, carbide, or an inter-metallic compound throughout a ductile matrix. For a given volume fraction of dispersed phase, strength is increased by decreasing the size and spacing of the dispersed particles.19&apos;20 Furthermore, room-temperature ductility may also be increased by changing the shape of a brittle dispersed phase from platelike to equiaxed or spheroidal.8 Overaging and redissolving of the secondary phase limit the maximum temperature to which precipitation-hardened alloys can be used. However, in a binary eutectic system, both phases coexist up to the melting point. Although all eutectic structures are not completely stable,21 a dispersion-hardened cast high-temperature alloy might result if a fine distribution of one of the eutectic phases could be obtained during solidification. An additional reason for interest in eutectic alloys is their excellent castability.22 Since eutectic alloys, like pure metals, freeze at a single temperature rather than over a range of temperatures, their castability is superior to solid-solution alloys with long liquidus to solidus ranges. The purpose of this research was to study the effects of small solute additions on the microstructure and mechanical properties of a number of high-melting-point eutectic compositions.

Jan 1, 1967

By L. Zwell, H. A. Wriedt

In describing their procedure for measuring the lattice parameters of solid solutions, Abrahamson and Lopata report (p. 77) the final heat treatment of their alloy specimens as "700°C for 100 hr, followed by a furnace cool". The isothermal part of this treatment may be expected to precipitate solute in excess of the stable a solid-solution limit at 700°C; the subsequent slow cooling is likely to reduce the dissolved solute still further. Fig. 1 (upper) presents the data for titanium alloys so he;rt-treated and shows the lattice parameters of solid solutions containing up to 3.5 at. pct Ti; Fig. 17 (lower) shows 2 at. pct Ti as the solubility limit in a iron at 700°C. Figs. 1 and 17 are thus incompatible. The paper contains comparable incon~patibilities for zirconium alloys, for niobium alloys, and for tantalum alloys. The final heat treatment at 700°C may also be responsible for the anomalous "knee" in the lattice-parameter data for nickel alloys, Fig. 3. The "knee" composition is located near the 700°C limit of the stable a solid-solution field;37 alloys of the experimental composition range with more nickel than the "knee" composition are two-phase at 700 C and prolonged heat treatment of them at 700°C would tend to produce inhomogeneity rather than homogeneity. In Figs. 4 and 7, the composition ranges of the zirconium, hafnium, and niobium alloys examined terminate at alloy concentrations of 0.1 to 0.2 at. pct. These metals form very stable oxides and their partial removal from solid solution in iron by impurity oxygen may be expected. We believe that the authors should have reported the procedure by which they distinguished the amounts of alloying elements in solution and in oxide. The diagrams pertaining to copper in Figs. 3 and 18 (lower) are almost certainly incorrect. Three recent investigations of this system38-40 all substantially agree on the solubility of copper in a iron, finding it to be much larger than that reported by Abrahamson and Lopata. The change of the lattice parameter with composition reported by Abrahamson and Lopata is too large by a factor of three to five, as seen by comparison with the findings of other investigators.41738 Moreover, the authors violate, in Fig. 18, the accepted Fe-Cu constitution diagram37 by ignoring the eutectoid at about 850°C.

Jan 1, 1967

By C. R. Johnson, R. A. Greenkorn, E. G. Woods

A new method of reservoir evaluation called pulse-testins has been developed for describing formation properties between wells. Pulse-testing utilizes a sensitive differential-pressure gauge at a responding well to measure and record the response generated by a series of flow rate changes (pulses) at an adjacent or pulsing well. Since the pulse-test instruments have a sensitivity of about 0.001 psi, pulses of several hours or less in duration will generate a measurable response in most reservoirs. For this reason, many well pairs can be tested in a short period of time with little interference in field operations. Comparison of pulse-test results to conventional testing methods shows that the pulses obey unsteady-state, compressible-flow theory and thus provide a measure of both transmissibility (kh/µ) and storage (Fch). In additian, the method can be used qualitatively to describe communication across faults and between zones, and direction and tnagnitude of fracture trends. INTRODUCTION To obtain maximum usefulness of new reservoir analysis methods as well as to aid the field engineer in understanding local reservoir anomalies, improved methods are needed to describe heterogeneities in specific reservoirs. Optimum well spacing, equipment specifications, well completion design and especially the economics of pressure maintenance and secondary recovery programs depend on the extent and location of the heterogeneities that affect flow behavior in the field. One method for obtaining a measure of areal reservoir heterogeneity is an interference test. In the simplest interference test. constant-rate production or injection is initiated at one well and the effect of this flow is measured as pressure vs time at another well. Thus, during interference tests the flow characteristics of the formation are determined in situ. Despite their obvious usefulness in reservoir delineation. interference tests have not enjoyed frequent usage. Reasons for this have been the weeks or months required in many fields to obtain a pressure response measurable with conventional gauges, and the interruption of routine field operation during the field-wide shut-in normally required during these long times. Also, only average properties of the relatively large volume of the reservoir disturbed during these long times can normally be obtained — variations in properties between individual wells cannot be delineated. To eliminate these drawbacks of conventional tests, a special reservoir description technique called pulse testing&apos; has been developed. Pulse-testing has several advantages that make it more convenient and practical for field use than interference tests. Valid tests are more certain because use of a series of flow disturbances gives rise to a diagnostic pressure response that can more readily be distinguished from unknown trends in reservoir pressure and other "noise." The time required is only a fraction of that for an interference test because a special, high-sensitivity differential pressure gauge can detect a much smaller pressure change. Variations in properties between individual wells can be delineated because of the relatively small volume of the reservoir disturbed during these short times. Finally, wells other than the pulsing and responding wells do not have to be shut in or carefully regulated.

Jan 1, 1967

By M. M. Singh, J. W. Brown

Three rocks of highly varied physical properties are selected for the first reported experimental study concerning microseismic activity of rock under tension to determine the effects of static fatigue, loading rate, repeated loading and rock anistropy compared to compression and bending loads. The microseismic method of detecting rock under deformation may be a great potential tool in surveillance and location in situ of dangerously stressed strata, as well as predicting rock failures. Noises emitted under load or the rate of energy (energy of noise pulses generated per unit time) are computed for varying conditions. The tests are conducted at constant load on a dead weight loading machine to eliminate all possible extraneous noises — an indispensable precaution — at various load levels. Experimental results are reported including the relation of total energy emitted to tensile strength of rock and the possibility of simulating a phenomenological model for microseismic activity. Plots of some of the experiments are included. INTRODUCTION Rock failure, whether on a large scale faulting in the earth&apos;s crust and rock bursts in mines, or on small scale ruptures of laboratory test specimens, generates transient vibrations in the rock mass. Mechanisms of intermittent deformation, such as twinning and cracking through and between mineral grains, also produce similar vibrations, but of very small amplitude. Such vibrations from both deformation and failure are referred to as microseismic activity, rock noise, or occasionally seismo-acoustical activity. An individual rock noise is sometimes

Jan 1, 1967

By L. N. Cosner, C. F. Austin, J. K. Pringle

Shock wave attenuation studies with three igneous rocks are reported: a spessartite elastic to low intensity stress waves, a diorite which is anelastic, and a porous scoria. The level of shock passing through a given thickness of rock has been determined by donor-receptor methods using high speed streak cameras. Test results include shock propagation velocities adjacent to the explosive, the dependence of test results upon test geometry, and the variation in shock wave attenuation in these three common igneous rock fabrics. The utilization of explosives in rock mediums involves a series of interrelated phenomena. These are the detonation process within the explosive, the transfer of energy from the explosion products to the surrounding rock medium in the form of sound or shock waves, and the transmission of the resulting waves through the rock medium to create damage in the rock mass. The subject of this paper is the investigation of the close-in phenomena that occur in the intensely shocked rock immediately adjacent to a detonating explosive charge. The specific aspects studied include propagation velocities, free surface velocities, pulse attenuations and the determination of the equations of state for the test rocks employed. In addition, a series of tests was conducted to indicate the dependence of the test results on the charge diameter utilized. The equations of state for rock materials have been investigated by a number of authors. Lombard, &apos;,&apos; Grine and Fowles,3,4 Zharkov, 5 Hughes and McQueen,6 Chabai,7,8 and Bass9 have published equation of state data on rock materials similar in structure or composition to those investigated in the study. Rinehart10 has prepared a voluminous tabulation of the available equation of state data from these publications and in addition has included data on many other rock and earth materials in his compilation. The reader is referred to the extensive tabulations and bibliography of Rinehart for classical studies involving the equations of state of metals and other solids and liquids. The problems of sympathetic detonation between drill holes in hard rock environments has received the attention of various authors as have the problems of explosive rock coupling close-in stress wave attenuation and explosive diameter effects. 11 to 18 In particular, the don or-receptor geometry of this report is very similar to the geometry of adjacent drill holes in rock. Most published pulse velocity and attenuation work in rock has been devoted to velocities at much lower amplitudes than those associated with close-in explosives phenomena and most attenuation studies involve transmission and attenuation across large spans of material. Excellent work in these areas has been published by the U. S. Bureau of Mines and by many individuals and groups engaged in geophysical research. SELECTION OF TEST MATERIALS A series of rock materials was desired for this test program that would be meaningful industrially, and that would also yield comparative results from a research viewpoint. Based on the availability of a series of related petro-fabrics, for which there is an abundance of physical and shock response data, three igneous rocks were selected as the test series. The applicability of shock wave studies in igneous rocks to industrial problems is readily demonstrated. Hardrock tunneling, quarrying and mining take place in igneous rocks throughout the world. From a research point of view, igneous rocks exhibit a wide variety of grain sizes and considerable diversity in composition, yet the common igneous rocks have a general similarity in their constituent mineral structures and in their grain-to-grain bonding mechanisms. The latter is based on the concept of rock formation through magma cooling and crystallization, though the degree of liquefaction in granitic plutonic masses is indeed a moot question. Three specific types of igneous rock were chosen for study. A coarse-grained granitic textured rock was desired that would serve as a representative of the widely abundant intrusive rocks of the world and

Jan 1, 1967

By J. W. Spretnak, J. N. Cordea

The gain boundary relaxation in high-purity aluminum, nickel, copper, and silver was studied by means of a low-frequency torsion pendulum. Both internal friction and creep at constant stress tests were conducted. A lognormal distribution in relaxation times was found to account for the relatively wide experimental internal friction peaks and the gradual relaxation behavior during the creep tests. This distribution was separated further into a lognormal distribution of relaxation time constants and a normal distribution in activation energies. A spread of up to ±6 kcal per mole in the activation energies accounted for the major part of the distribution. A "double-peak" internal friction phenomenon was observed in silver. The activation energies in kcal per mole derived from the grain boundary relaxation phenomena are 34.5 for aluminum, 73.5 for nickel, 31.5 for copper, and 41.5 for silver. It was found that the rain boundary relaxation strength in these metals increases with the reported stacking-fault energy. GRAIN boundary relaxation phenomena have been observed in a large number of polycrystalline metals and alloys. Numerous investigations have been conducted to study the structure of the grain boundary through this relaxation process. One of the first investigators was Ke1-4 who observed that the activation energy for grain boundary relaxation in aluminum, a brass, and a iron was about the same as that for volume diffusion. He concluded that the grain boundary behaved as if it were a thin liquid layer with neighboring grains sliding over one another. Leak5 conducted experiments on iron of a higher purity and observed that the grain boundary activation energy is comparable with that of grain boundary diffusion. He suggested that, in metals where this relationship holds, the damping may be caused by a reversible migration of grain boundaries into adjoining grains. Nowick6 has presented an interesting view of inter-facial relaxation with his "sphere of relaxation" model. A relaxed interface is represented as one where the shear stress is greater than the normal value along the edges and zero in the interior of the interface. The region of the stress relaxation is pictured as a sphere surrounding the interface. From his calculations Nowick concluded that the slip along an interface is directly proportional to its length. Therefore, the time of relaxation, T, depends on the size of the relaxation interface. This means that in the Arrhenius relationship, t = TO exp[H/RT], valid for atom movements, the relaxation time T is predicted to be proportional to the grain diameter through the pre-exponential term, TO. Since the internal friction can be given as Q-1 = ?j wt/(1 + w2r2), where ?J is the relaxation strength and w is the angular frequency, an increase in grain size at a constant frequency will shift the peak to a higher temperature. A great deal of work has been done to determine the exact relationship between the internal friction and grain size.1,5,7,8 In metals, the grain boundary peaks are found to be lower and broader than predicted theoretically.&apos; The above model can explain this by a distribution in the size of the interface areas, represented by a distribution in the parameter tO, and an overlap of spheres of relaxation, represented by a distribution in activation energies. Both these phenomena result in an over-all distribution in the relaxation time, which could affect the internal friction peak height, breadth, and also position. This relationship between the experimental data and theoretical calculations appears very promising in the study of interfacial relaxation mechanisms. THEORY A lognormal distribution in t can sometimes be used to adequately describe the spectrum of relaxation times governing an anelastic relaxation. wiechert9 originally suggested such a distribution to explain the elastic after-effect in solids. This choice is particularly applicable to grain boundary relaxation when considering Saltykov&apos;s work.&apos;&apos; He found a lognormal distribution in the grain sizes within a metal. Recently Nowick and Berry11 have introduced a log-normal distribution in T into the theoretical internal friction equations. The form of the distribution function is where z = In(r/rm), and Tm is the mean value of t. The parameter ß is a measure of the distribution and is the half-width of the distribution when is l/e of its maximum, IC/(O). Nowick and Berry have described the methods to obtain the parameters Tm, ß, and ?,J from experimental internal friction and creep test data. In the idealized case, where only one relaxation event occurs with one relaxation time, only ?J and T are necessary to completely describe the event, and 0 = 0. For the broader internal friction curves 6 is some positive number greater than zero. The larger the 6, the greater is the half-width of the distribution in In t.

Jan 1, 1967

By Emmanuel P. Papadakis

Ultrasonic velocity measurements have been made to study the preferred orientation in cube-textured copper. Methods applicable to thin specimens were employed since the specimens were necessarily of sheet material. The measured velocities in various directions in the sheet differed from the corresponding values in single-crystal copper by 1 to 6 pet. The distribution of the deviations indicated that the align-ment of the (001) planes with the rolling plane was better than the alignment of the [100]and [010] directions with the rolling and transverse directions. Ultrasonic pole figures (velocity us orientation) are shown to be useful in the study of preferred orientation. THIS paper describes one set of experiments in a continuing study of preferred orientation in worked metals. This study has been undertaken to investigate the fundamental properties of metals when used as propagation media for ultrasonic waves. Many such materials are of current or potential use in ultrasonic delay lines. Fundamental studies on ultrasonic propagation parameters such as velocity, attenuation, and diffraction (beam spreading) are of importance in the design of delay lines, in the development of nondestructive testing methods, and in the study of materials themselves. Preferred orientation in worked poly-crystalline metals influences all three above-mentioned parameters, and hence is of particular importance. When polycrystalline metals are subjected to mechanical working, they develop textures dependent upon their crystal structure and the symmetry of the working operation.&apos; The texture consists in the alignment of the crystallographic axes of the grains in preferred directions with respect to the symmetry axes of the working operation. Since the grains are elastically anisotropic, the elastic moduli of worked metals are anisotropic. Hence the velocities of elastic waves in worked metals depend on the directions of propagation and polarization. The worked metal may be thought of as taking on the elastic symmetry of a single crystal: so it possesses the same number of independent elastic moduli as the crystal class it simulates. In general, a worked metal does not adopt the crystalline symmetry of its own grains. For instance, most rolled sheet becomes effectively orthorhombic while all bar stock and wire develop hexagonal symmetry. However, certain metals with cubic crystal structure develop a cube texture upon rolling and annealing.= Nearly perfect alignment of [100]-type directions with the rolling direction, transverse direction, and rolling-plane norma1 can be achieved in certain fcc metals and alloys. These cube-textured rolled metals provide an excellent opportunity to test preferred orientation by means of elastic waves, since a worked metal with 100 pct cube texture would have elastic moduli identical to the moduli of its constituent metal. It is the purpose of this paper to present the results of an investigation upon cube-textured copper. Ultrasonic waves were used. The methods of measurement and the experimental results on the effective moduli will be given. The ultrasonic measurements will be shown to complement X-ray pole figures for the determination of preferred orientation in worked metals. EXPERIMENT To study cube - textured material, it was necessary to use thin-sheet material since a severe reduction in gage (95 to 99 pct) is necessary to produce cube texture. Special ultrasonic methods were needed to investigate the thin material at megacycle frequencies. A) Materials. The cube-textured material tested was a copper alloy containing 1 pct Zn. Specimens already measured for Young&apos;s modulus4 by Alers were kindly supplied by him. The specimens were slabs 3.00 by 0.25 in. cut from sheet 0.047 in. thick. The orientations of the long axes of the specimens with respect to the rolling direction were taken in 15-deg steps from 0 to 90 deg. B) Measurements. Two distinct experiments were performed to measure the phase velocity in these specimens. One measured the shear wave velocity for propagation in the 0.25-in. direction and polarization in the 3.00-in. direction. The other measured the velocity of both shear and longitudinal waves propagating in the thickness direction in the sheet. 1) Plate-Mode Measurements. The velocity of the zeroth-order shear mode5 was measured in the 0.25-in. direction in each strip. The specimens were ground thinner over half their length to assure that the first-order shear mode would be cut off below 6 Mc per sec, leaving the zeroth-order nondispersive shear mode as the only propagating mode. Piezoelectric ceramic transducers of 5 Mc per sec resonant frequency poled in their long direction were solder-bonded to the edges of the thin part of the slabs as in Fig. 1 after these edges had been made flat and parallel by fine grinding. These transducers produced waves polarized in the 3.00-in. direction and propa-

Jan 1, 1967

By Yoichi Ishida, Ching-Yao Cheng, John E. Dorn

Tile creep behavior of a iron was investigated over the range of temperatures from 375° to 1150°K. Apparent activation energies for creep, obtained by the effect of sudden changes in temperature on the creep rate, revealed the presence of- four distinguishable regions. The creep behavior of a iron in Regions II (480° to 774°K) and 111 (775° to 1045°K) was found to correlate well with a model where the creep rate is controlled by the nonconsevualive motion. of jogged screw dislocations. An anomalous increase in the apparent activation energy fur creep in Region III was found to be in harmony with the known decrease in the free activation energy for self-diffusion over the Curie transformation range. Furthermore, the creep rates in Regions II and III were found to increase with stress due not only to the effect of stress on the activation energy but also to an increase in density of mobile dislocations. The evidence suggests that pipe diffusion along moving dislocations could be a significant factor over the lower temperatures of Region II. ALTHOUGH the creep properties of iron and steel have been of interest to metallurgists for some time and an extensive literature is now available, most of the published information has not produced much toward understanding the fundamental dislocation processes controlling the creep behavior of these materials. Whereas the activation energy for high-temperature creep of metals usually agrees well with that for self-diffusion, Sherby, Orr, and Dorn1 deduced from the data of Tapsell -and c1enshaw2 that the activation energy for creep of Armco iron is about 78,000 cal per mole and more recently Lytton and sherby3 reviewed the data of Jenkins and Mellor4 and found an activation energy for creep of a iron of 80,000 cal per mole. Both values are substantially greater than the activation energy for self-diffusion in a iron. Because of the limited data suitable for purposes of identifying the controlling dislocation mechanisms of creep and the unusually high activation energies for creep quoted above, it was considered desirable to reinvestigate in detail the creep of a iron by more reliable techniques which would provide sufficient data for determination of the creep mechanisms. EXPERIMENTAL TECHNIQUE Creep specimens were prepared from 3/8 by 4 in. iron bar stock of the following composition by weight percent: 0.001 C, 0.0120 0, 0.001 N, 0.004 S, and 0.003 P. The as-received bars were cold-rolled to a thickness of 0.100 in., annealed under argon for 30 min at 1113°K, cold-rolled to a final thickness of 0.063 in., and machined into tensile specimens having gage section 0.250 in. wide and 1.70 in. long. Finally they were recrystallized under argon at 1113°K. Specimens to be crept above 1060°K were recrystallized at 1173°K. Both recrystallization treatments gave the same reproducible equiaxed ASTM No. 4 grain size. Creep testing was conducted in machines fitted with Andrade-Chalmers arms that maintained a constant stress to within ±0.2 pct of the reported values. Deformation over the specimen gage section was sensed with a linear differential transformer and recorded auto-graphically as a function of time. The strains deduced from these measurements were sensitive to ±5 x 10-5. During creep the specimens were contained in an argon-filled chamber which was immersed in a temperature-controlled molten tin bath. Creep temperatures, as measured by thermocouples attached to the specimen, were maintained to within ±10.25°K of the reported values. For activation-energy determinations rapid changes in temperature of about 12°K were obtained within 30 sec by direct resistance heating of the creep specimen, and maintained to ±1°K of the reported values. Observations of structural details of specimens before and after creep tests were made by electrolytic polishing and etching in acqueous ammonium persulfate. EXPERIMENTAL RESULTS A typical example of the determination of apparent activation energies, Q, by the effect of small changes in temperature is illustrated in Fig. 1. Q is defined by

Jan 1, 1967

By Donald B. Hunter

The Ti-Be system up lo 10 wt pct Be with cortlmercialll&apos; pure titanium has been determined using metal-lographic techniques. Beryllium forms the p eutec-toid type of dinqarz with titanium; the eutectoid occurs at 0.5 xt pct Be azd 1500 F, while an eutectic is foritled at 1887°F containing between 5 and 7.5 rt pct Be. The solubility of beryllium in a titanium does not exceed 0.05 zvt pct and the maximum solubility of Beryllim in 0 titanium is 1 wt pet. PREVIOUS work on the Ti-Be phase diagram indicated that additions of beryllium to titanium resulted in a marked lowering of the melting point,&apos;&apos;&apos; and it was also observed that the solubility of beryllium in both a and p titanium was retricted.- With the limited data available, McQuillan and McQuillan constructed a partial hypothetical diagram of the Ti-Be system,= assuming that beryllium formed the 0 eutectoid type of system with titanium. Subsequently Bedford published a tentative diagram of the entire Ti-Be system: although he did not investigate alloys containing less than 10 wt pct Be. This diagram included several compounds described by other authorities.&apos;-l3 The following account describes work directed toward determining the form of the titanium-rich portion of the phase diagram up to 10 wt pct Be. MATERIALS AND METHODS Titanium sponge and a master alloy containing 25 wt pct Be were used in the formulation of the alloys; the chemistry of these materials is detailed in Table I. The alloys were prepared as 250-g compacts which were melted into buttons by arc melting under purified argon on a water-cooled copper hearth. Results of analyses for beryllium are shown in Table I but no determination of other elements was made at this stage. The alloys were hot-rolled at 1650°F to produce 0.1-in.-thick sheet. Alloys containing up to 1.5 pct Be were fabricated without trouble; samples containing 2 pct cracked initially upon hot rolling, but thereafter rolled satisfactorily to sheet. The 5, 7.5, and 10 pct were hot short and could not be rolled. Surface contamination was removed from samples by sandblasting and pickling in a 5 pct HF-35 pct HNOs solution. For metal log raphic examination, heat-treated specimens were mounted transverse to the rolling direction, ground on silicon carbide papers of increasing fineness to 600 grit, and electropolished at 20 v using a solution containing 600 ml of methanol, 60 ml of perchloric acid, 360 ml of butyl cellosolve, and 2 ml of Solvent "X". Difficulty was experienced in obtaining good electropolished surfaces with samples containing more than 1 pct Be, the degree of difficulty in-

Jan 1, 1967