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By J. Brett, L. Seigle, L. Castleman, T. Montelbano

Impurity-induced low-temperature recrystallization of cold-worked tungsten was inuestigated with emphasis on the influence of nickel on the reaction. Palladium, nickel, aluminum, manganese, platinum, and iron greatly lower the recrystallization temperature of doped tungsten, which zs normally very high, but the recrystallization temperature of electron-be am zone-refined tungsten wzre is slightly raised by conlacl with nickel. Recrystallization can be induced at low temperature by the presence of solid nickel on the surface of doped tungsten wire, but apparently not by exposure to nickel vapors alone. Approximately 200 ppm of Ni dijjused into 10-mil wires at 1200 from a deposit of nickel on the surface produced total recrystallization, whereas more than 600 ppm of Ni could be absorbed frotn a vapor source without altering the fibrous structure of cold-worked tungsten. Once initiated, nickel-induced recrystallization required a continued source of' nickel for propagation of the recrystallization front. The solubility of nickel in fibrous 10-mil W wire was approximalely 500 ppm at 1150' C, and the activation energy for penetration of the recrystallization front was 52 kcal per mole. In many applications the usefulness of tungsten depends on critical control of its structure. Cold-worked tungsten with the fibrous structure developed by suitable thermo-mechanical treatment has a low, but technologically significant, ductility. It has long been known1 that traces of nickel, and perhaps other metals, are profoundly deleterious in doped tungsten, because they induce recrystallization at low temperature, which produces a brittle, equiaxed grain structure. This effect appears to be an exception to the general observation that recrystallization is impeded and the recrystallization temperature raised by the presence of impurities.2"9 Previous studies7-'' of the annealing and recrystallization of tungsten wire have divided the phenomenon into prior recovery stages, primary recrystallization and secondary recrystallization. The present investigation is concerned principally with primary recrystallization which is defined here as the replacement of the fibrous structure of deformed tungsten by equiaxed grains. The objective of this study was to explore the nickel-induced recrystallization reaction in tungsten and attempt to elucidate its mechanism. As well, an effort to define which other elements give rise to low-temperature-induced recrystallization was carried out. EXPERIMENTAL PROCEDURE The procedure adopted for these experiments was essentially to bring nickel and other elements into diffusive contact with cold-worked tungsten wires. The process of recrystallization was followed as a function of time and temperature by light and electron microscopic observations. First the influence of nickel on the recrystallization temperature of arc-melted, zone-refined, and variously doped tungsten wire was determined by electroplating a deposit of nickel on the surface of the wire and annealing at a variety of temperatures for 3 hr. The chemical analyses of the tungsten wires used in this investigation are given in Table I. The surface of the tungsten wire was etched with Murakami's slution' and approximately 0.005 in, of Ni was deposited from a Watts-type low pH bath14 for the conditions of these experiments. Variations in plating thickness from about 0.001 to 0.005 in. had no discernible influence on the resulting structures. The wires were then annealed in an atmosphere of dry hydrogen to establish the recrystallization temperature. Concurrently, un-plated specimens were annealed to establish the recrystallization characteristics of nickel-free wire. The criterion of recrystallization was that the fibrous structure be completely replaced by equiaxed grains after a 3-hr treatment of temperature. This provided more reproducible results than use of the first recrystallized grain or a fixed proportion of re-crystallized structure as the critical observation. The structures encountered in longitudinal and transverse sections were examined by both light and electron microscopy at magnifications up to X32,000 using parlo-dion-carbon replicas shadowed with platinum for the latter method. Second, the influence of a variety of metals on the recrystallization temperature of 0.010 in. D alumina-silica doped tungsten wire, AW136-64, was determined. The elements were applied by electroplating whenever possible. Alternatively, they were vapor-plated on the tungsten wire and a greater thickness built up by coating with a dispersion of metal powder in nitrocellulose lacquer. Elements not amenable to either of these procedures were merely slurry coated on the tungsten. The recrystallization temperature was determined as above. Third, the nickel-induced recrystallization process in doped wire was studied more closely by electroplating 8 mils of Ni on 65-mil alumina-silica doped tungsten wire, AW153-NS10, and exposing the wire to temperatures of llOO°, 1200°, or 1300°C for various times in a hydrogen atmosphere. A circular recrystallization front, 'Onsisting of equiaxed grains, developed at the periphery Of the coated tungsten wire, and the advance of this front into the fibrous interior was studied. These experiments employed relatively coarse 0.065 in. D wire because the 0.010 in. D wire recrystallized too quickly to permit observation of the pene-

Jan 1, 1969

By W. D. Sylwestrowicz

In tests on polycrystalline copper and aluminum, the ratio of the yield stress to modulus of elasticity was found to be strongly dependent on tempemture. Also, it was shown that the change of the yield stress with temperature of a material at a given temperature and deformed to a given yield stress, but not necessarily to the same strain, does not depend on previous mechanical thermal history. Likewise, for a material at a given temperature and deformed to a given yield stress, the rate of work hardening is independent of the temperature of prior stressing. It has been shown by Los and Orowan1 and by Dorn, Goldberg, and Tietz2 that the temperature dependence of the yield stress-strain curves of crystalline materials reflects two effects: not only does the yield stress of a material in a given structural state depend on the temperature, but the structural state (and the corresponding strain hardening) after a given amount of plastic straining also depends on the temperature at which the pre-straining has been carried out. Thus, for instance, if a specimen of a ductile metal has been strained along the stress-strain curve 1 at room temperature to point A, Fig. 1, and then the straining continued in liquid nitrogen along curve NR, the yield stress A' immediately after lowering the temperature is lower than the yield stress A" of a specimen that has been strained by the same amount in liquid nitrogen (along curve 3). AA' represents the effect of the temperature change upon the yield stress of the specimen pre-strained at room temperature; A' A" is the excess strain hardening acquired if the pre-straining has been carried out in liquid nitrogen instead of at room temperature. The dependence of the yield stress (i.e., of the structural state acquired during preceding straining) upon the conditions (speed, temperature) of a pre-straining is the reason for the nonexistence of a so-called "mechanical equation of state" for plastic deformation. A 'mechanical equation of state" is a relationship of the form F(s,E, e, T) = 0, or s = f(E, E, T) [1] It was first suggested by Ludwik3 that plastic deformation might obey such an equation; this, however, was conclusively disproved by experiments of Kochendorfer.4 Additional disproofs were given in

Jan 1, 1959

By G. R. Hodgson, M. P. Lebourg

The introduction in the field of a new type well completion called for the setting of tubing open-ended in the well before perforating the casing. This paper describes a new perforating tool of the shaped charge expendable type, small enough to pass through tubing and powerful enough to perforate the casing. The perforations are produced at an angle and are large enough for optimum production. Performance of this tool in targets and under various well conditions is described. Very often no lifting equipment will be available at the well. In some cases, pressure will exist in the well at the time of the perforating operation (workover wells or multiple trip perforation) ; therefore, new equipment and new technique for the perforating operation were devised. This paper describes this equipment and technique, particularly casing collar recording, sheave support, and cable pull-down device. this last item being necessary for wells under pressure. Results obtained with this tool in the field are given. INTRODUCTION One of the key requirements for the introduction in the field of a new method of permanent well completion was the development of a new perforating method involving the use of a perforating gun small enough to go through tubing and with enough penetrating power to perforate the casing satisfactorily. The equipment described in this paper was basically designed to go through open-ended two-in. tubing and to perforate 5 1/2 in. casing. The equipment is illustrated in accompanying figures. NEW COMPLETION METHOD With the new permanent type well completion, the production string of casing is run and cemented through the potential producing zone. Open-ended tubing is -then run into the well and used to replace the drilling fluid with oil or water. The amount of the oil or water "cushion" can be varied according to the expected bottom hole pressure. Thus, if desired, the hydrostatic head can be greater, equal to, or less than the expected pressure within the zone to be perforated. Mud having been displaced, the tubing is -then positioned so that the end is above the zone to be perforated. The Christmas tree and flow lines are installed and tested. The drilling rig can now be removed from the well since it is not necessary for the perforating operation, thus resulting in a saving in rig tme. The perforating equipment is then moved to the well and the gun lowered through the tubing. After the gun passes out of the open end of the tubing, the depth measurements are correlated with casing collars and the gun placed opposite the zone to be perforated. Upon firing, the gun body is shattered and falls to the bottom of the well. Since the lubricator has been closed before firing, it is possible to withdraw the casing collar locator and head and then open the well immediately to the tanks. DESCRIPTION OF GUN An investigation of two basic types of Perforators, namely a bullet perforator and a shaped charge gun, was undertaken towards the development of a gun to meet the aforementioned requirements. Preliminary tests on various bullet perforator designs within the diameter limitations did not give results encouraging enough to warrant further study. Somewhat better results were obtained by using conventional shaped charges; but, as in the case of the bullet types, the necessarily small overall diameter proved to be a severe limitation and resulted in insufficient penetration. A shaped charge employing a new design was developed which gave excellent penetration. These shaped charges were designed to produce a large hole directed upward at a 45" angle. In order to obtain the maximum space possible for these charges, it was decided to use an expendable carrier made of drillable material, usually aluminum, which would shatter at the time of firing, leaving only harmless fragments at the bottom of the hole. The fixed spacing is five shots per ft. wit11

Jan 1, 1952

By Maurice Ewing, A. P. Craby, J. W. Peoples, J. A. Peoples

The purpose of this paper is to present the results of the application of the earth-resistivity method of subsurface investigation to the problem of locating seams of anthracite coal beneath a mantle of soil and subsoil. Details are given of the successful use of this method in locating the outcrops of anthracite seams in actual prospecting. The presence of the outcrop of an anthracite seam is indicated at points where electrical resistivity tests showed relatively low readings. The reason for this is that in some localities the resistivity of anthracite was found to be about 0.0001 megohm-cm. compared to 1 to 200 megohm-cm. for shales and sandstones. For two reasons it is believed that the data summarized in this paper should be of particular interest. In the first place, most of the interpretations of the resistivity survey have been checked by subsequent drilling and some by the removal of the overburden and the exposing of the anthracite seams. It is infrequent that the opportunity for checking results so thoroughly is given. In the second place, the fact that recent commentatorsl,2,3 on the application of geophysical methods to mining have concluded that direct prospecting for anthracite and other types of coal is not promising makes the good results obtained more significant. So far as the authors can learn, the only previous experiment with electrical methods in the Pennsylvania anthracite field was one made by Sherwin F. Kelly in 1921, when he used the self-potential method at Wilkes-Barre4. The profile he made does not show a very marked correlation with the geologic cross section. Kelly points out that stray currents from electric motors in the mines undoubtedly affected 'his results, but the experience of the present authors with stray currents from mining machinery suggests the possibility that the potentials measured by Kelly were due almost entirely to this effect.

Jan 1, 1936

By R. S. Craig, W. E. Wallace, G. S. Kamath

The destruction of long-range order in Mg-Cd, has previously been thought to occur as a second order process. In the present work a variety of X-ray diffraction techniques are employed to show that in this case and in Mg-Cd alloys containing frorn 20 to 33 1/3 at. pct Mg the process more nearly resembles an ordinary first order phase transformation. It is found that the ordered alloy, which occurs as a single phase at lgw temperatures, transforms with increasing temperature into a Cd-enriched disordered (P) phase and an Mg-enriched ordered (a) phase. The interval over which these two phases coexist under apparently equilibrium conditiovs extends from 25" to 87°C content. At 33 1/3 at. pct Mg the two-phase region has disappeared. Measurement of the long range order parameter, s, for the ordered phase in MgCd, (from superlattice line intensities) shows that it disorders only very slightly before it is transformed into the p form. Kinetic experiments reveal that when the a phase is formed frorn the p phase by suitably quenching so as to suppress phase segregation, the transformation is essentially complete and the a phase has acquired its equilibrium value of S in less than 1 min. In an earlier investigation carried out in this Laboratory1 the rate of disordering of the MgCd3 superlattice was determined over an extensive range of temperature. The process was found to be first order and the rate constant, k, was established. At the lowest temperatures studied k was found to increase exponentially with temperature. At higher temperatures, however, it passed through a maximum and for the 100 deg interval below the point at which the superlattice was destroyed k was observed to decrease with increasing temperature. The various theoretical treatments1-3 of order-disorder phenomena lead to a negative temperature coefficient for k near the superlattice critical temperature but this region for MgCdB seemed unusually wide. Detailed analysis of the point indicated' that either the long-range order parameter, S, for MgCda varied with temperature in an anomalous way or the disordering in this instance is more complex than in the cases which have been treated theoretically. The original objective in the present work was simply to determine S vs temperature for MgCda to ascertain whether the disordering was in conformity with theoretical expectations.2° In an early stage of the work it was noted, however, that under equilibrium conditions ordered (a) and disordered (0) phases coexist in MgCd, over a considerable range of temperature. Since on thermo- dynamic grounds the coexisting phases must differ in composition, the investigation was enlarged to permit the compositions of the two phases in MgCd3 to be determined and to establish the extent of the two phase regions for alloys containing from 20 to 33 1/3 at. pct Cd.

Jan 1, 1963

By F. E. Jaumot, R. L. Smith

Self-diffusion in zinc has been used as an instrument for comparison of the absorption and sectioning techniques as a means of studying diffusion. Single crystal as well as poly-crystal samples were used asanda the temperature range of diffusion extended from 200° to 415°C. For temperatures above 200°C, the data indicate that the results obtained from the absorption technique agree with those obtained from the sectioning technique. The effect on the values of the diffusion coefficient of electroplating vs evaporation as a means of applying the tracer was investigated and no significant difference observed. It was found that an excess or deficiency of tracer did not materially affect the results obtained from the sectioning technique, but invariably caused errors with the absorption technique. NEARLY all self-diffusion experiments and many alloy diffusion experiments have employed radioisotopes as the instrument for following the diffusion. Of the various techniques in which radioisotopes are applicable, the two most widely used are the sectioning and absorption techniques. In the former, the diffusion coefficient is obtained from a curve of log concentration vs the square of the mean penetration depth. In the latter, the diffusion coefficient is calculated from a knowledge of the decrease in activity at the surface after diffusion. In spite of the importance of knowing the reliability of the diffusion data and the widespread use of these two techniques, they had not been directly compared experimentally on the same samples. Thus, such a comparison was worthwhile. The specific system chosen for this comparison was the self-diffusion of zinc, since the metal was readily obtainable in high purity, single crystals were easily grown, and the anisotropic features of the diffusion added an additional factor of interest to the comparison. Self-diffusion in both single and polycrystals was investigated, since the possibility existed that grain boundaries and grain boundary diffusion might produce different effects for the different techniques. Also, the effects of electroplating vs evaporation as a means of applying the radioactive tracer, and the effects of applying an excess or deficiency of tracer material were studied. The general experimental procedures and the mathematical analyses of both techniques have been described previously in some detail, and only those points essential to an understanding of the present work will be discussed here. The mathematical analysis of the sectioning data requires only a knowledge of the solution of Fick's equation. where C,, is the initial concentration, C is the concentration at depth x, D is the diffusion coefficient, and p is the absorption coefficient of the solvent metal for the radiation from the solute. Having obtained F from the experiment, the value of z can be read from a plot of F vs In z, and D can then be calculated if is known. The necessity of knowing the absorption coefficient causes most of the criticism of the absorption technique. It is very difficult to measure accurately under the conditions existing in the diffusion experiment, but it is absolutely necessary, as will be indicated briefly later. Portions of this problem have been discussed in detail elsewhere." The difficulties involved in the measurement of the absorption coefficient arise from three principle factors: the physical characteristics of the absorber, the geometry, and complex radiation spectra. The first two are heavily dependent upon the third. If

Jan 1, 1957

By J. D. Price, G. V. Woody

MANY producers of by-product coke have spent considerable time and given considerable thought to the use of a substitute for low-volatile coal as an admixture with high-volatile coking coal for charging high-temperature by-product coke ovens. Generally speaking, there are two principal reasons for this, one being occasioned by the lack, in certain localities, of low-volatile coal delivered at a cost sufficiently low to permit its use, and another being the desirability of finding a substitute product with a delivered cost lower than the cost of the low-volatile coal. It was for the first of these reasons that the Colorado Fuel and Iron Corporation was particularly interested in this subject. This paper deals with the experimental work and the results obtained by that company in producing and using low-temperature char. OVERCOMING DEFECTS IN COKE FROM COLORADO COALS Colorado coking coals are all of the high-volatile type and were all laid down during he Cretaceous period, which makes them something like 80 million or so years younger, geologically, than eastern coals. They behave, when coked alone, something like the Pittsburgh-seam coals. They make a very brittle, highly cross-fractured, fingery coke of fair shatter value but quite low in resistance to abrasion. Mixed with a low-volatile coking coal such as Pocahontas or certain Oklahoma coals, they make a coke that is equal to virtually any of the eastern cokes. The inferior quality of Colorado coke has long been recognized, and a considerable amount of time, effort and money has been spent upon investigations of means for improving its physical properties. While it has been found that some improvement in quality of coke can be secured by the adjustment and control of such variables as pulverization, moisture content, oven temperature and bulk density of charge, and through the addition of certain inert materials such as pulverized coke breeze, pitch, high-volatile noncoking or semicoking coal, the benefits so gained have been comparatively small. There are no low or medium-volatile coking coals available within a reasonable freight-cost distance. Therefore a substitute for low-volatile coal was developed through low-temperature carbonization-or, more correctly speaking, through the partial devolatilization-of high-volatile coals. The blending of this lower volatile char with the high-volatile coking coal distinctly improves the quality of coke made from Colorado coal. There is nothing especially new about this idea. In 1908 a Japanese patent was taken out by Kotaro Shimomura, whose claim was: The method of making a nonfingery coke out of bituminous coals, without using natural coals of low-volatile matter; according to which a certain coal is heated at a temperature between about 300°C. and about 600°C. so as to leave about 15 to 25 per cent volatile matter in the coal; this coal is mixed with the

Jan 1, 1944

By F. J. Fayers, R. L. Perrine

For many years the problem of increasing ultimate recovery of oil from a reservoir has been a subject of interest to the oil industry. At present, a standard secondary recovery technique is to flood the reservoir with water once natural forces of the system are depleted. The permeability characteristics of the rock, together with interfacial forces which exist between the two fluids and the porous material. allow only part of the oil in the rock formation to be recovered by the water-flooding process. Laboratory experiments have shown that when detergents are added to the flooding water, the flow properties of oil in a porous rock arc improved. This improvement results in greater oil recovery. Even though higher recoveries are obtained using detergents, the extra cost associated with the method may make it economically unsatisfactory. To establish economic feasibility requires experimental laboratory measurement of fluid and rock properties together with a calculational procedure to predict field results. Pilot tests in the field may also be required. This paper presents a mathematical procedure for predicting detergent flood behavior. A number of reasonable simplifying assumptions are made to obtain a tractable system of equations. The resulting method may be regarded as a generalization of Buckley-Lev-crett' theory to solve simultaneously for water saturation and detergent concentration profiles. Consequently this type of calculation can be used in much the same manner as Buckley-Leverett theory is used to evaluate a water flood. The mathematical method employed is the so-called method of characteristics for solving hyperbolic partial differential equations. This application of the method is instructive because several other problems in reservoir analysis may be analyzed in a similar manner. FLUID FLOW EQUATIONS The flow behavior of oil and water without detergent through porous reservoir rock is usually expressed by Darcy's law and a continuity equation for each phase. If gravitational forces are neglected, vrg = kr (s)µr v p rg.........(1) vrg = kr (s)µr v p rg.........(1) ? pa va = F ?/?t (sd) where v is the volumetric flux, k represents permeability, S is saturation, and P the pressure. Fluid viscosity is denoted by 11, p is the density, 4 is porosity, and I the time. The subscripts w and o refer to water and oil. The capillary forces in the system lead to a difference in pressure between phases. This may be expressed by the relation: Pm -P0 =Pc(S).........(5) The capillary pressure? P,, is determined experimentally as a function of saturation. DETERGENT BALANCE EQUATION Addition of detergent to the water phase affects the flow properties of the system. Capillary pressure and relative permeability become functions of detergent concentration, c, as well as fluid saturation. That is: P--P (S,c) and k,,,.- - -- k,,,. At low oil saturation values, the presence of detergent reduces capillary pressure and reduces the relative permeability ratio. Detergents are surface-active and adsorb on rock surfaces. The quantity adsorbed, a, will depend on the concentration c of detergent solution and may also depend on the saturation; thus, a = a(S,c). In this analysis we have assumed that the detergents used are water soluble but not oil soluble, and their movement is therefore restricted to the water phase. The dispersion of detergent in water is neglected by comparison with transfer by flow within the system. Detergent movement is determined by the water flux and adsorption: ? cv m = -F ?/?t (cs + a) We will assume that the quantity of detergent in solution is too small to significantly change water density or viscosity. When the permeability and capillary pres-

By E. C. Harder, D. F. Hewitt

Since early in 1916, when it became apparent that the steel industry of the United States could not depend for the duration of the war on several important foreign sources of manganese and might have to depend entirely on domestic ores, the U. S. Geological Survey, with the assistance of several cooperating organizations, has made a comprehensive investigation of domestic manganese resources. The work has included field studies in a number of states well as annual, quarterly, and monthly canvasses among operators concerning current and future production. In order that the interested public might have access to the important results of the studies, preliminary reports concerning the field work as well as periodic summaries of production were issued as promptly as possible. Although numerous summaries of production l2, l3, l4 have been prepared from time to time for the use of the several boards and committees responsible for the conduct of the war, it has been thought for some months that those engaged in the industry, as well as others, might be interested in a preliminary summary of the accumulated geologic and production data. The cessation of hostilities, in November, 1918, probably detracts from the usefulness of much of the material that is here presented, but apart from the historic interest in the performance of an important industry in war time, there is a possibility that some of the conclusions may be helpful to those who continue to exploit domestic deposits, as well as to those who wish to measure the country's independence in mineral supplies. Appropriate final geologic reports are being prepared by the geologists who did the field work. The present authors, having done but a small part of the recent field work, acknowledge with great appreciation the use of preliminary and unpublished reports and the cordial informal cooperation of the following geologists in the preparation of this paper: F. L. Ransome, G. W. Stose, F. C. Schrader, J. T. Pardee, E. L. Jones, Jr., H. D. Miser, Laurence LaForge, J. B. Umpleby, Arthur Keith, F. J. Katz, and E. S. Larsen, of the U. S. Geological Survey. Field work in Virginia was carried out in cooperation with the Virginia Geological Survey, T. L. Watson, State Geologist; in Georgia, with the Georgia

Jan 1, 1920

By H. A. Meyerhoff, R. J. Colony

Deposits of iron are widely scattered in the folded Cretaceous rocks and the associated igneous intrusives of Puerto Rico. Most of them are too small for commercial development, but a few have aroused some scientific and economic interest, among them the large body of residual limonite at the west end of the island near Mayagüezl-6 (Fig. 1) and the mixed hematite and magnetite deposit on the southern slopes of the Sierra de Cayey, about four miles north of Arroyo.7"9 Neither of these orebodies has been developed, nor have investigations of the widely distributed deposits of magnetite, which include all the remaining occurrences of iron deserving of economic consideration, proceeded beyond the exploratory stage. With the possible exception of the mixed deposit near Arroyo, the magnetite is directly associated with andesitic and dioritic intrusives, which invade the Cretaceous rock section, and the bulk of it, occurring in calcareous sediments, is clearly of contact-replacement origin. The small deposit on Rio Portugües, north of Ponce, is found in a limestone band near its contact with an andesite dike.10,11 Two deposits of unde-

Jan 1, 1935

By John E. Greenawalt

In view of the increasing importance of sintering in the beneficiation of iron ores preparatory to their reduction in the blast furnace, the writer believes the time is opportune for an up-to-date, though brief, discussion of the general principles of sintering, as well as a discussion of some of the recent improvements and mechanical developments that have been achieved in this industry, its present trend and future possibilities. Sintering may be defined as the agglomeration of fine mineral particles into a porous mass by incipient fusion caused by heat produced by combustion within the mass itself. Its first successful application, in connection with the treatment of lead sulphide ores, was known as blast roasting. In this process the lead ore was given a preliminary roasting in a reverber-atory furnace, then the incandescent mass was placed in a pot with a grate and an updraft was applied. It was soon discovered that much better results were obtained by cooling the ore, moistening it, and placing it upon an incandescent layer of fuel previously placed upon a grate, and then applying the updraft blast of air until the charge was converted into a more or less agglomerated mass. The fuel was sulphur and the process one of desulphurization, which was the principal result desired. The application of downdraft to blast roasting brought about tremendous results; the principal one of which was that an air blast of high pressure could be passed through a layer of ore deposited on a grate, or on a grate covered by a layer of coarse porous material, without disturbing the particles of which the layer is composed. The air current is compelled to filter through the pores of the charge, whereas if the same pressure applied to the top surface of the charge with downdraft were applied to the bottom of the charge with updraft, the charge would be completely blow11 off the grate. Another result of reversing the draft was that a flame could readily be applied to the top surface of the charge for igniting purposes. Broadly speaking, sintering is an oxidizing or burning process, therefore the volume of air passing through the charge is the all-important factor. The air must pass through with sufficient rapidity to produce the necessary heat, and if sufficiently rapid the combustiorl will take place

Jan 1, 1938

By A. A. Scheil, S. I. Hoyt

In technological studies on steel considerable emphasis has been placed on the identification of the foreign inclusions, testimony of which is adequately given in the metallographic literature covering methods for their identification. The outstanding accomplishment in this field is the scheme devised by Campbell, Comstock and Wohrman for identifying various oxides, sulfides, silicates and other constituents by systematic etching tests and microscopic examination.' The time involved in carrying out this procedure has led to attempts to secure quicker methods, or at least to shorten the time required to secure essential information. An example of this is the use of dark field illuminatin,2 but when this was tried out by the authors it was found that cavities and pits on the polished surface appeared bright on a dark field and could not be distinguished from small glassy inclusions. Still another means is the Leitz Ultropak, an instrument equipped with optical units for the illumination of the specimen by reflected light to secure an effect similar to dark field illumination. The structures are made visible in exceedingly sharp details by utilizing the inherent properties of the samples, such as refractive index, absorption coefficients and reflection powers. We have had no experience with the Ultropak, but a recent paper by Benedicks and Löfquist3 describes methods for determining the refractive index of (Fe, Mn) O and MnS by the use of this equipment. Presumably this method would be subject to about the same limitations as dark field illumination, though the, feature added by Benedicks and Löfquist appears to offer great promise in inclusion identification.

Jan 1, 1935

By Albert A. Smith

The creep properties of metals have assumed increasing importance in recent years and many investigations have been made on various phases of the problem. In the past year the annual lectures of the Institute of Metals Division1 and the Iron and Steel Division2 were concerned with this subject, and are excellent reviews. For many years the creep properties of lead and lead alloys have been investigated at the Central Research Laboratories of the American Smelting and Refining Co., and it is hoped that the present paper will contribute knowledge of some of the factors that influence creep. Lead, being a metal that recrys-tallizes readily at room temperature, is an excellent material upon which to investigate creep phenomena because of the simplicity of the apparatus needed, and it might be expected that results would apply to some extent to elevated-temperature tests of other metals. Material The creep tests of this investigation were all made on high-purity lead (99.9998+ Pb) in which the only impurity that could be detected by spectrographic and chemical means was approximately 0.0001 per cent Fe. Flat strips, 0.750 in. wide by 0. 100 in. thick, were prepared by extruding 2-in. dia. cast billets at a temperature of 250°C. This gave a material of 2 to 3 mm. average grain size with a tensile strength of j.400 lb. per sq. in. when tested at a straining rate of 5 per cent per minute. With this extremely soft material, great care was necessary in handling the specimens, to avoid distortion and subsequent recrystallization. The creep tests at 30°C. were conducted in a constant-temperature room, specially built for the purpose in the basement of an office building in which there was no moving machinery, and no vibration was detectable under the most severe conditions of shock in the adjacent surroundings. The room was well insulated and heated electrically, control being by means of a de Khotinsky regulator operating a relay. Maximum temperature variation over a period of several years has been ± 1/2°C. Specimens of the extruded strip, 16 in. long, were used for test purposes with no reduced gauge section, thus eliminating any distortion due to machining. The method of clamping and supporting the specimens is shown diagrammatically in Fig. 1. The gauge marker for the measurement of extension consisted of an aluminum strip, 0.050 in. thick by 0.75 in. wide, one end of which was ground and sanded to a precise knife-edge and fastened to the specimen by suitable pins. After the strip was fastened in place a fine scratch was inscribed just below the knife-edge by means of a sharp teasing needle. Just below this gauge scratch a short vertical mark was made so that the same point could be located and read each time. Several hundred specimens have been prepared by this method, and it was found that with experi-

Jan 1, 1941

By J. B. Morgan

The mechanical behavior of MgCu2 from 20 o to 725°C has been determined by "brittle-ring" tensite-test techniques, axial compression, and bending experiments. Compressive ductility begins at 450°C (0.65 T/Tm) and slowly increases with increasing temperature white the tensile ductility is characterized by an abrupt brittle-ductile transition at 600°C (0.8T/Tm). The compressive strength increases eightfold from room temperature to 400°C with a "normal" decrease as the temperature is further increased. The tensile strength goes through a rather abrupt threefold increase above 600°C with a subsequent decrease at higher temperatures. The slip system is (111)[110] and the twinning system is (111)[112]. At high temperatures MgCu2 is quite rate-sensitive, and dynamic yield points are observed that are extremely orientation-dependent. The high-temperature creep behavior under constant load is characterized by an increasing strain-rate with time. The general characteristics of the mechanical behavior make it possible to classify MgCu2 with those materials in which initial mobile dislocation density and the dislocation velocity-stress dependence are significant in determining mechanical response. Mgcu2 is the C15 prototype of the cubic Laves phase. Its range of homogeneity extends from 32.8 to 35.5 at. pct Mg at 500°C and narrows at lower temperatures. The lattice parameter is reported to vary from 7.02 to 7.05A,1 and the compound is completely ordered to the melting point of 819°C. MgCu2 has a brassy metallic appearance, is extremely brittle, and many of its physical properties are intermediate between those of the constituent elements: the electrical resistivity is 3.5 x 10-6 ohm-cm, Young's modulus is 10x 106 psi, the shear modulus is 6 x l06 psi, and the thermal coefficient of expansion is 18.7 x 10-6 cm per cm per "C from 20" to 250°C. Usually, properties of intermetallic compounds as functions of temperature have been determined by hardness, compression, or impact behavior, and almost all of these experiments have been performed on polycrystalline materials. Tammann and Dahl,2 for instance, determined the onset of ductility in a series of binary intermetallics by ball-hardness measurements and found the onset to range between 0.71 and 0.96 T/T,. Lowrie's3 investigations included some tensile properties, and he found ductility beginning around 0.65 T/Tm for most materials examined. His work did include some data on polycrystalline, nonstoichiometric MgCu2, however. The present work is an attempt to extend the examination of the particular compound MgCu2 in single-crystal form in order to aid the formation of general concepts about mechanical be-

Jan 1, 1965

By B. J. Shaw, R. Kossowsky, W. C. Johnston

High purity (99,95) Ni-51 wt pct cr eutectic alloy was unidirectionalty solidified at rates of 0.1 to 8 in. per hr. The resulting material was characterized by large grains, approximately 0.5 mm in cross section and extending through almost the entire length of the specimen, parallel to the growth axis. The eutectic structure of specimens the growth at -1/3 The per hr consisted of a continuous nickel-rich phase and chrome -rich lamellae approximately 2 thick, spaced about apart. Specimens were tested in compression at temperatures ranging from —196 to 850"C over which range the 0.2 pet yield strength dp -creased from 160,000 p si to 35,000psi, respectively. Swaging to 40 pet reduction in area, followed by a 30-min anneal at 1000c to remove residual cold work, increased the 0.2 pet yield to 260,000 psi at -196°C, dropping to 35,000 psi at 850°C. The increase in strength was attributed to a residual cell structure. The strength of the alloy could be rationalized by the simple rule of mixtures if one assumed that additional strength is derived front a size effect characterized by is petch equation IN recent years there has been increasing interest in dispersion and second phase strengthening in materials needed for high-temperature applications. inm role of structure on the mechanical The of such alloys has been well established of such some extent accounted for theoretically. and to of how the strengthening mechanisms due to fibers and lamellae operate has been reduced to its fibers form by the fabrication of composites of strong rods unidirectionally aligned in a From work on tungsten-fiber-reinforced copper, for example, it was established that the "Rule of Mixtures" could explain the strengthening.12 " some what more sophisticated technique for introducing strong fibers into copper matrix was used by Hertzberg strong Kraft3 who unidirectionally solidified the copper-chromium eutectic. The use of unidirectionally fied eutectics has advantages in that there are no matrix-fiber wetting problems and fine fibers are automatically aligned and uniformly fiber However, one Is restricted to a specific volume fraction of the second phase. Nevertheless, even though the volume fraction is fixed, the rod or lamella thickness, , can be varied by controlling the freezing interface velocity. Alternatively, the grown material may be worked down by swaging or rolling. Embury and Fisher, " using this approach, drew down pear lite in iron and studied the mechanical properties iron and that the yield strength, oy, was properties.proportional They that d was the wire diameter. It could be inferred that was also proportional to but the work hardening had to be taken into consideration at the same time. By varying the growth rate of the cadmium-zinc lamellar eutectic, Shaw'1 showed that was proportional to without the introduction of work hardening and suggested that the lamellar interface itself contributed to the strengthening of the composite. In this investigation we have evaluated the mechanical properties of the unidirectionally solidified fec-bec eutectic Ni-Cr. This eutectic was selected because it presented the possibility was selected beca temperature, and high corrosion resistant alloy, and also represented a hard-soft phase combination with two completely different slip systems. Specimens were tested in compression and tension up to 850°C and a detailed study of the micro structure as a function of plastic strain and temperature was carried out by light and electron microscopy. It was shown that the composite strength tested in compression can be accounted for by the simple rule of mixtures if one allows for an additional term representing the effect of Intereprese EXPERIMENTAL PROCEDURE 1) Unidirectional Solidification. Fig. 1 is a schematic drawing of the apparatus used to produce 0.2 in. diam by 12 in. long alloy ingots. The crucible tube is alumina, containing the charge which has been is swaged, or machined to 0.195 in. diam. The lower end of the tube is immersed to 0 .195in in.d iam. The upper end is supported by a 10 mil nichrome wire which lowers the crucible mil nic hr the] wire at a prescribed rate. Surrounding the furnace is a graphite susceptor into which a control thermocouple is inserted. The furnace is insulated with fiberfrax and enclosed in a quartz tube. There is a sliding seal at the bottom around the crucible and one on the top so that an atmosphere may be used for the sample and suscep tor. The power for the furnace is supplied from a 10-kw, 450 kc generator. The skin depth (the skin depth at which the field falls to l/e of its value at the outer surface) for graphite (p = 10 (j-ohm-cm) is 0.1 in. at this fre-

Jan 1, 1970

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.' 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'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 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 H. I. Aaronson, C. Laird

The kinetics of thickening and of lengthening of ?' plates in an Al-3.93 pct Cu alloy in the temperature range 203" to 300" C were determined by means of transmission electron microscopy. The rate of thickening was found to be less than that allowed by volume diffusion control at all temperatures, by amounts which increased with decreasing temperature, in agreement with the predictions of a general theory of precipitate morphology.1 Thickening was treated on the basis of the ledge mechanism. Ledges were deduced to spread across the broad faces of ?' plates at volume dzjrfusion-controlled rates, as anticipated from the disordered structure of their edges. Lengthening of 8' plates, on the other hand, took Place more rapidly than allowed by volume dzjrfusion. This occurred despite clear morPhological evidence of a bmrier to growth at the edges of these plates. It was concluded that the misfit dislocation structure comprising the barrier requires that lengthening take place by a jog mechanism. The tnisfit dislocations, however, also serve as diffusion short circuits, and allow high overall lengthening rates to be achieved. In Part I' it was shown that, within the range of aging temperatures and times studied, the broad faces of 8' plates formed in Al-4 pct Cu are fully coherent with the a, matrix. Virtually .all of the dislocations present in these faces were found to have developed as a result of plastic deformation in the a phase. Such dislocations are thus "intruders", rather than the more usual misfit-compensating variety. The edges of 8' plates were confirmed, by extension of the earlier studies of Mat-suura and Koda,3 to be made up of edge-type misfit dislocations, in sessile orientation with respect to lengthening of the plates. These interfacial structures should cause 8' plates to thicken and to lengthen at rates less than those allowed under the condition of volume diffusion control, such as would be expected if the interphase boundaries had disordered structures.' The narrow width of 8' plates, the reproducible crystallography of their broad faces, and the appearance of these plates in cross section as octagons rather than as circular discs2 provide qualitative support for these deductions. The present study of the rate of thickening and the rate of lengthening of 8' plates was undertaken in order to examine them on a quantitative basis. I) THICKENING KINETICS OF THE BROAD FACES OF?' PLATES A) Literature Review. The measurements now available on the thickening kinetics of single-phase precipitate plates consist of one plot of the thickening of a proeutectoid ferrite plate in an Fe-C alloy,' showing (as predicted) thickening rates less than those allowed by volume diffusion control. B) Experimental Procedure. Details of the preparation of the 4-3.93 pct Cu alloy used in this study have been previously reported.4 As in Part 1,' transmission electron microscopy was the observational tool employed. A general description of the apparatus and procedures of the electron microscopy studies is given in Section I of Part I. In thin foils, 0' plates tend to form at and parallel to the foil surface.' A direct investigation of the thickening process by means of hot-stage transmission electron microscopy was therefore not feasible. It was thus necessary to use the conventional method of aging individual bulk specimens for a wide range of different times at the various temperatures studied. In each specimen, the thicknesses of a number of plates were measured. Since thin foils prepared from "bulk-aged" material contain a large proportion of grains with orientations near (001) , it was relatively easy to find, near the edges of the foils, the characteristic multifold patterns of intersecting extinction contours which indicate regions where the foil is exactly at an (001) orientation. The thicknesses of large numbers of plates were measured along the (200) branches of the "stars" so that the 8' plates were precisely parallel to the optical axis of the microscope. Wherever possible, intersecting extinction contours were adjusted with the parameter s > 0 to improve the visibility of the plates in bright-field illumination. These precautions, in combination with taking the measurements at the thinnest parts of the foils, minimized the errors in the measurement of the thickness of the plates resulting from inexact parallelism to the electron beam. Since the plates were very thin, it was not easy to measure their thickness on the photographs. The techniques of enlargement and of microdensitometry were employed to minimize errors from this part of the measurement. A further source of possible error, that the plates can appear thicker because of contrast associated with mismatch normal to the plane of the plate, was also considered. The images of the plates were usually thinner than those of dislocations, however, and no anomalous changes in apparent plate thickness were observed when regions of foil containing plates were tilted through various diffracting conditions. Any error from this cause must therefore be small. Other sources contributing errors were: a) the microdensitometer traces per se and the subjective estimates of their peak limits, and b) slight fluctuations in magnification associated with small changes in the current of the objective lens of the electron microscope. The overall error probably amounted to no more than 5 to 10 pct. In order to obtain readily interpretable data on thickening kinetics, it is essential that the diffusion fields of adjacent ?' plates not be allowed to overlap. Calculations'-' showed that this condition is definitely not ful-

Jan 1, 1969

By G. H. Gronhovd, W. H. Oppelt

Complete gasification to produce synthesis gas for manufacture of synthetic chemicals and fuels offers possibilities for utilization of the vast lignite fuel deposits in the U.S. The design of a slugging, fixed-bed, pressure gasification pilot Plant is described. Results are presented for initial operation of the plant at moderate pressure and using low-temperature char as fuel. Gasification of solid fuels is becoming increasingly important in the future overall energy picture, both in this country and abroad. Snythesis gas from gasification of coal consists chiefly of carbon monoxide and hydrogen, and after suitable purification and modification this gas can be used in the production of synthetic ammonia, methanol, higher alcohols, and synthetic liquid fuels, or as a reducing gas in the metallurgical field.' Most synthesis gas used in this country is made from natural gas, petroleum oils, and refining tail-gases, but the direct gasification of coal will become more attractive as costs of petroleum oils and natural gas increase.' A gasification process designed for use with brown coal and lignite was developed by the German Lurgi Co. prior to World War 11. In this process a fixed bed of lump-sized fuel is gasified with steam and oxygen at pressures ranging from 370 to 440 psi. Effective heat exchange between the ascending high-temperature gases and the descending solid fuel results in low gas outlet temperatures, high thermal efficiency, and favorable oxygen consumption. Lurgi gasifiers are used commercially for the production of synthesis gas or as a substitute for coal gas in many countries, including Germany, Czechslovakia, Great Britain, South Africa, Australia and Pakistan.3-6 The chief disadvantage of the conventional Lurgi gasifier which operates under nonclinkering conditions is that large quantities of excess steam must be supplied with the oxygen-steam mixture to reduce the temperature in the fuel bed below fusion temperature of the ash. Most of the steam leaves the gasifier undecomposed with the product gas and, after cooling, produces large amounts of dilute liquor. Evaluation of fixed-bed gasification experiments using dry-ash removal indicated that by increasing the oxygen concentration in the oxygen-steam blast the temperature in the combustion zone could be raised high enough to operate under slagging conditions. 7-8 Operation of a fixed-bed pressure gasifier under slagging conditions would reduce the steam requirements and the volume of waste liquor and would increase the steam decomposition, the overall thermal efficiency of the process, and the rate of gas production per unit cross sectional area of the gasifier. Because the Lurgi gasification process, modified for slagging operation, offered possibilities for efficient gasification of American lignite, the Bureau of Mines decided to investigate the process on a pilot-plant scale at the Grand Forks, N. D., Lignite Research Laboratory. DESIGN Description of Pilot Plant: A flowsheet of the Grand Forks slagging gasification pilot plant is presented in Fig. 1. The gasifier unit consits of the coal lock, the gas generator, and the slag lock. The fuel, which is periodically charged to the coal lock, moves by gravity flow into the generator and is continuously gasified by an oxygen-steam mixture introduced at the bottom of the gasifier. Molten slag is formed at the hearth and flows through a central taphole into a water quench bath. The slag-water slurry is periodically discharged from the slag lock. Process steam is generated and superheated in separately-fired, oil-burning units. Oxygen is supplied to the gasifier from a gas storage bank located some distance from the pilot plant. The capacity of the oxygen storage bank is about 130,000 standard cu ft at 2200 psig. Liquid oxygen is delivered by truck and is converted to gas during the filling operation. The superheated steam and oxygen are metered separately, then mixed and fed to the gasifier tuyeres. The gas generator is surrounded by a water jacket. The steam formed is separated in the steam drum and then discharged to the gas offtake, thus equaliz-

Jan 1, 1961

By F. Weinberg

It has been suggested, for some time, that the behavior of metals under high-temperature creep conditions is strongly influenced by the behavior of the grain boundaries present in the material. This has led to a number of investigations1-6 in which attempts were made to measure the properties of the grain boundaries themselves, both to determine their contribution to the creep process and to obtain further knowledge of their intrinsic structure and properties. The present investigation was undertaken to extend the observed data under more closely controlled experimental conditions and to attempt to clarify sonie of the discrepancies in the literature. A brief report of the preliminary results has been published.7 EXPERIMENTAL PROCEDURE For the present investigation, controlled orientation specimens were used having plane boundaries which terminated at the specimen surface. Trierys-tal specimens were used instead of the bicrystal type of Puttick and King,' in order to simplify the gripping technique required to apply a shear stress along the boundary. The aluminum used was obtained from the Aluminum Francaise and was of 99.994 pct purity, containing 0.002 pct each of Cu, Fe, and Si. The aluminum tricrystals were grown horizontally from the melt, in graphite boats, and in an argon atmosphere, following the technique developed by Chalmers.' The orientation of the tricrystals was controlled by using seed crystals separated by mica inserts. Thermal conditions were adjusted to produce tricrystals having boundaries which were macroscopically straight, parallel to the growth direction, and perpendicular to the top surface. Following growth, the tricrystals were carefully cut with a jeweller's saw to the test specimen shapes shown in Fig. l(a) and l(b). In Fig. 1(a), the boundaries subjected to shear stresses are indicated AB and CD: Points A and C are the ends of the mica inserts separating the seed crystals; points B and D are at lateral cuts made in the specimen. It was found that the slots left by the mica inserts at A and C had to be enlarged slightly, by cutting, to ensure that the boundary terminated freely at these points. A shear stress was applied to the boundarks by gripping the upper two legs in file-faced Inconel grips and suspending a weight from the lower part of the specimen held in similar grips, as shown schematically in the diagram. The test specimens shown in Fig. 1(b) were cut from long

Jan 1, 1959