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By Klaus Detert, Joseph Ziebs

The progress of primary recrystallization has been studied in alloys of nickel with 0.01, 0.1, and 1.0 at. pct Ta. It can be shown that in one particular alloy containing 0.1 Ta and 0.02 02 a large grain structure (0.5 mm diameter) could he developed by primary recrystallization in thin sheetswhich were cold-worked to 97.5 pct reduction in thickness. Electron transmission microscopy demmstrates that this phenonmena was linked to the occurrence of fine precipitates at subboundaries. A discussion of how fine precipitates can exert under certain circumstances a rather distinct retarding effect on nucleation rate is included. IN a former investigation, the recrystallization and texture formation in a series of binary nickel alloys including pure nickel were studied.' Nickel alloys with some tantalum added displayed peculiarities during primary recrystallization which have been studied in more detail by the present investigation. The alloys were prepared by powder-metallurgy techniques similar to the previous investigations.' Pure metal powders were thoroughly mixed to obtain alloys with 0.01, 0.1, and 1.0 at. pct Ta, referred to as alloy A, B, or C, respectively. The metallic impurities were kept below 0.005 at. pct except iron and cobalt with slightly higher values, by using highly purified nickel and tantalum powders.' The mixtures were pressed into bars and sintered at a temperature of 1300°C. The sintering atmosphere was either high vacuum, dry hydrogen, or wet hydrogen. The sintered rectangular bars were rolled 60 pct to a thickness of 3 mm, then annealed under dry hydrogen at 1000°C and again cold-rolled to about 97.5 pct reduction of thickness. After this heavy deformation, the sheet thickness was 0.07 5 mm. In order to study primary recrystallization which occurred in measurable times between 400" and 600°C, samples of the rolled sheets were annealed in a salt bath at various temperatures for various times in order to study the progress of recrystallization by hardness measurements and microscopic examination. For optical observation, the samples were polished and etched in a solution of 65 cu cm HNO3, and 18 cu cm acetic acid in 20 to 100 cu cm H2O, depending of the particular sample and annealing treatment. For transmission electron microscopic observations, thin foils were prepared by the combined window and Bollmann techniques.273 The electrolyte consisted of 23 pct perchloric acid and 77 pct acetic acid held at 15°C. Polishing was performed at a current density of 0.4 amp per sq cm. The examination of the thin films was accomplished by a Siemens Elmiscope-type electron microscope operating with an accelerating voltage of 100 kv. RESULTS The progress of primary recrystallization was very accurately followed in these alloys in order to establish the time when recrystallization started and ended during an isothermal anneal. Table I gives some of the data obtained by these studies. The time for beginning is a mean value, where somewhat less than 5 pct of the matrix has recrys-tallized. The end of recrystallization is the time when at least 95 pct of the matrix has recrystal-lized. Listed are three different B alloys, with 0.1 Ta distinguished by different sintering atmospheres which influence the rate of primary recrystallization. By the above method, the state of the grain structure when primary recrystallization was completed, but grain coarsening had not started, could be clearly defined. The average grain diameter of the recrystallized matrix is also given in Table I. The grain size did not depend on the temperature of the isothermal anneal. With one exception the grain size of the primary recrystallized matrix was found to be rather fine

Jan 1, 1965

By P. S. Kotval, H. Hahell

PRECIPITATION of M23C6 carbides at grain boundaries in austenitic steels and nickel base superalloys has received considerable attention. Hatwell and Berghezan,1 in a study using carbon extraction replicas, observed that dendritic growth of the M23C6 carbide phase occurred at grain boundaries in austenitic steels. Merrick and Nicholson2 have observed that in thin foils of "Nimonic 75" alloy the precipitation of M23C6 carbide was discontinuous at grain boundaries. Lewis and Hattersley3 have suggested that the type of M23C6 precipitation observed in Ni-Cr austenites represented the early stages of discontinuous precipitation. In a more recent study, Singhal and Martin4 have concluded that grain boundary M23C6 precipitation involves the migration of an austenite grain boundary by a mechanism very similar to that proposed by Tu and Turnbull.5 Tu and Turnbull's suggestion essentially involves grain boundary migration under the driving force arising from the difference between the surface free energies of the opposite sides of the plate. Thus, Singhal and Martin's observation4 implies that the first stage of discontinuous precipitation has taken place and that the grain boundary has provided a diffusion short circuit for the sub-stitutional solute atoms (principally chromium) which assist the preferential growth of the M23C6 plate in contact with the grain boundary. However, no evidence of the characteristic cellular morphology typical of discontinuous precipitation was found in Singhal and Martin's studies. Presumably, this is due to the low volume fraction (i.e., low supersaturation of solute) of the precipitating carbide reported by Singhal and Martin.4 Recently, Raymond6 has studied precipitation of the M23C6 carbide in Incoloy alloy 825 and shown that the growth of this phase is perpendicular to grain boundaries at 1400°F and in the plane of the grain boundary at 1700°F. The former aging condition resulting in discontinuous or "cellular" precipitation. Raymond has suggested an explanation for this behavior based on the relative rates of chromium diffusion by volume and grain boundary diffusion at the two different aging temperatures. In the course of a recent investigation on precipitation behavior in several ' strengthened superalloys, precipitation of M23C6 carbide at grain boundaries was studied. Under conditions of a high degree of supersaturation, the M23C6 carbide precipitates in the discontinuous or cellular morphology in Waspalloy (Ni-18.51 Cr-2.0 Fe-3.53 Mo-1.16 Al-2.78 Ti-0.09 C). This note presents electron microscopy observations of this mode of precipitation and its effect on mechanical properties. Specimens of Waspalloy after "solution" heat treatment at 1950°F show essentially single phase matrix with a few residual particles of "primary" MC carbide. In normal commercial heat treatments, precipitation of Ni3(Al,Ti) ordered fcc r' phase occurs throughout the matrix and M23C6 precipitates as globular particles at the grain boundaries. In these commercial heat treatments the degree of supersaturation during precipitation is low. However, if specimens of Waspalloy are quenched from the solution heat treatment temperature of 1950°F and then aged at an aging temperature where the degree of supersaturation is high, discontinuous precipitation of M23C6 occurs. Figs. 1 and 2 show thin foil micrographs of Waspalloy, solution heat treated at 1950°F, water quenched, and aged at 1292° and 1598°F, respectively, for 500 Fig. 1—Thin foil of Waspalloy, solution heat treated at 1950°F for 1 hr, water quenched, and aged for 500 hr at 1292°F. Magnification 15,500 times. Fig. 2—Thin foil of Waspalloy, solution heat treated at 1950°F for 1 hr, water quenched, and aged for 114 hr at 1598° F. Magnification 13,000 times.

Jan 1, 1970

By Y. C. Liu, G. A. Alers

measurements of the anisotropy in Young's modulus produced in copper by rolling 95 pct reduction in thickness below room temperature have been carried out in order to study the dependence of the texture on rolling temperature. The results clearly show the transition from a copper-type texture to a brass-type texture as the temperature of rolling is lowered. The intermediate textures observed can be described very well as a simple mixture of the two terminal textures. These results cormbined with other texture measurements make possible afresh review of the experimental facts velating to rolling textures in fee metals and, as a consequence, a critical examination of the current theories is presented. PREVIOUS experiments have shown that the transition from the copper- to the brass-type rolling texture is clearly displayed and can be quantitatively analyzed by measurements of the anisotropy of Young's modulus.' Application of this method to the Cu-Zn alloy system showed that the description of the texture transition as a gradual rotation of the grains from the orientation characteristic of the copper texture to the {110}(112) texture of brass2 was inconsistent with the data. Instead, the data suggested that the texture within the transition region could be described as a simple mixture of the two terminal textures.5 Unfortunately, it was difficult to establish this point conclusively because of the inadequacy of corrections for the composition dependence of the single-crystal elastic constants. Since a rigorous establishment of the nature of this texture transition is essential to our understanding of the formation of rolling textures in fee metals, it is clearly important to undertake an investigation in which the composition dependence of the elastic constants would not enter. A suitable composition-independent texture transition is provided by the well-established variation in the rolling texture of copper with rolling temperature. This temperature-dependent texture transformation has been studied by smallman' in several fee alloys and by Müller5 and others"' in copper. They observed that the texture characteristic of copper rolled at room temperature changed to a brass-type texture when the rolling temperature was lowered to 77°K. Although it is not possible to decide unequivocally from the published pole figures whether or not the 77°K rolling texture of copper is entirely of the brass type,' this complication does not affect the main purpose of the present investigation. In addition to establishing the nature of the texture within the transition region, the modulus data should also provide a determination of the temperature at which the transition occurs as well as the temperature range over which the transition extends. This information when combined with the modulus data on Cu-Zn alloys would then provide a considerable body of new information on textures in fee metals. Since these modulus results and the data obtained from pole-figure studies must be internally consistent, it is appropriate to compile a brief summary of the experimental observations based on all available methods rather than on the pole-figure data alone as has been done in the past. The primary purpose of such a summary would be to yield a more precise definition of the experimental facts on the rolling textures of fee metals, and thus greatly facilitate our evaluation of various proposed theories in this field. The final section of this paper is devoted to this compilation of consistent, experimental facts and their application to the various theories. EXPERIMENTAL PROCEDURE Two 18-lb ingots of cathode copper of 99.99 pct purity were induction-melted under a nitrogen atmosphere in a graphite crucible and chill-cast into a steel mold. The ingots were repeatedly cold-rolled and annealed (I hr at 500°C) into slabs about 1 1/8 in. thick. Blocks 3 1/4 in. wide, 2 1/4 in. long, and 1.000 in. thick were machined from each slab. The rolling schedule used was the same as in the previous investigation1 and the final thickness of the sheet was 0.050 in. with a rolling reduction of thickness of 95 pct instead of 97.5 pct as in the previous work.' The compositions and temperatures of the cold baths used for the low-temperature rolling were as shown in Table I. After each pass the rolled strip was immediately immersed in the cold bath for about 1 min or until the bubbling of the bath had subsided. The modulus data were taken within 2 hr after the rolled strip was warmed to room temperature for the first time, so that effects due to recrystallization were minimized. The modulus specimens were in the shape of flat bars, 3 in. long, 4 in. wide, and 0.050 in. thick, cut with their long dimensions oriented at 15-deg intervals between the rolling direction and the transverse direction. The values of Young's modulus were deduced from measurements of the frequency at which these long narrow bars were set into longitudinal, resonant vibration as previously described.9 To excite the mechanical vibrations in the specimen, an electromagnetic drive similar to that employed by Thompson and lass" was used. The maximum in the amplitude of

Jan 1, 1968

By R. L. Sandefur

Professor Kim's excellent review article1 on ultimate pit planning contains a statement of the apparently widely held but incorrect belief that "kriging provides information on the confidence limits around the estimate which no other extension technique is capable of supplying." If a geostatistical approach is valid, there are several good reasons for using kriging but uniquely provided confidence limits is not among them. If kriging is possible, then confidence limits can be calculated for any other linear estimate.

Jan 6, 1979

By T. K. Redden

Protective coatings based on the formation of a surface coating of nickel aluminide (NiAl) were applied to the nickel-base superalloys IN 100, SEL 15, and U-700. Coated specimens were exposed to an oxidizing environment at temperatures between 1600 and 2200 F for times up to 1000 hr. The oxidation resistance and stability of the coating were evaluated by weight gain measurements, metallographic examination, and X-ray diffraction study of surface oxides and coating. The composition of the coating and diffusion zone was determined by electron microprobe traverse of samples before and after high-temperature exposure. Intermediate phases formed in the coating and diffusion zone were identified by X-ray diffraction in situ and after electrolytic extraction. The outer coating was found to consist of the inter-metallic compound, NiAl, while the diffusion zone contained MC, M23C6 or M6C carbides, and a phase in a matrix of NiAl + Nidl. Oxidation resulted in formation of an A1203 n'ch scale containing some Tz02. Depletion of aluminum during oxidation resulted in degradation of the outer coating to Ni3Al and the nickel alloy matrix. Diffusion of aluminum into the base metal was found to be slight and did not influence coating life significantly. The o formed in the diffusion zone during coating decomposed during elevated-temperature exposure to form stable carbide phases characteristic of the base metal. Diffusion zone phase changes were found to have no effect on the life of the aluminide coating in the oxidizing envzron?nent. THE oxidation resistance of many high-strength nickel-base superalloys is inadequate for extended exposure at temperatures above about 1600°F. In addition, some applications for these materials require that they be exposed to environments containing sulfur compounds and sodium salts which can cause surface attalk known as sulfidation or hot corrosion. In order to provide the necessary corrosion resistance to the high-strength alloys, protective coatings based on an aluminizing process have been developed. These processes, usually based on a pack cementation technique, result in the formation of a NiAl-rich outer coating layer either during the coating process or by a subsequent diffusion treatment. The performance of the aluminide coatings is affected by interactions between the coating layer and the base metal both during the coating process and during subsequent exposure at elevated temperatures. Knowledge of these interactions is required to guide the development of coatings capable of longer life and improved reliability. Goward et al.' recently reported the metallurgical factors which influence coating per- formance on MAR-M200. The present work is concerned with correlating the interactions and performance of coating compositions on several representative materials. EXPERIMENTAL PROCEDURES Materials. Three cast nickel-base superalloys which are used for turbine buckets in air-breathing engines were studied: IN 100, U-700, and SEL 15. Their chemical compositions are given in Table I. The alloys were vacuum-induction-melted and cast to slabs approximately 0.3 in. thick from which rectangular specimens 0.25 by 0.5 by 1 in. were machined. Coating Procedures. The machined specimens were coated by CODEP processes which were developed at the author's laboratory. These are based on pack cementation in various media to deposit either aluminum or aluminum in combination with titanium. The coating process which deposits only aluminum is designated CODEP-C, while the CODEP-D process deposits titanium in combination with aluminum. The CODEP-D process was applied only to IN 100. Both CODEP processes are applied at 1950" or 2000°F for 4 hr without need for a subsequent diffusion treatment. An outer coating about 1 mil in thickness is produced by these processes. Test Procedures. Coated specimens were exposed to static oxidation for periods ranging from 24 to 1000 hr at temperatures of 1600" to 2200°F. Terminal weight gain measurements and visual examination were used to evaluate oxidation resistance. including oxide spalling and coating failure. Both as-coated and exposed specimens of each alloy were studied by metallographic examination, electron microprobe analysis (EMA), and X-ray diffraction analysis either of the exposed surfaces or of phases extracted from the coating and diffusion zone. RESULTS As-Coated Condition. The microstructures of as-coated conditions were generally similar, irrespective of base materials or the particular coating process. They are typified by IN 100 coated by CODEP-D as shown in Fig. 1. The predominately single-phase outer layer, area A, Fig. 1, was identified by X-ray diffraction as the intermetallic compound NiA1. The NiAl zone extended inward to the original base metal interface. The diffusion zone, area B, Fig. 1, included carbide phases, a lamellar phase oriented perpendicular to the base metal surface, and a matrix phase consisting of a mixture of NiAl and Ni3Al. The phases in the diffusion zone were electrolytically extracted using a 10 pct HCl in methanol solution at approximately 1.3 amp per sq cm. The extracted phases were found to be M6C, MC, or M=C6 carbides and o as shown in Table I1 for each of the alloys. The d spacings from a typical diffraction pattern are

Jan 1, 1969

By S. A. Hoenig

In an earlier publication, the application of exoelectron technology to the monitoring of dry grinding in a ball mill was reported. Recently, the author has investigated the ball mill problem in more detail with the system shown in [Fig.1]. Here, some of the current generated in the ore-ball-water mixture was picked up by the metal chains and served as a measure of the rate of grinding. While the mechanism of current generation has not been completely clarified, a parallel study of electrical effects associated with rock drilling indicated that the major driving force is the zeta potential*, while oxidation of the freshly fractured material provides the remainder of the current. Both of these effects are sensitive to the exposed surface area, and it might be expected that the observed currents would provide a measure of the grinding rate. This "surface area" effect allows the measurement system to be used in any type of rock or ore grinding. Some studies with sulfide copper ore indicate higher currents than those observed with silica sand, but the overall pattern of current versus grinding rate is essentially the same. Experimental Studies The experimental system was set up as shown in [Fig. 1]. The initial studies were done with silica sand because of its availability and for comparison with the data of reference 1. The sand was sized to an average of 425 /MI (40 mesh); a typical charge consisted of 2.5 kg (5.5 lb) of sand, 0.85 L (0.22 gal) of tap water and 2.5 kg (5.5 lb) of iron grinding balls 25.5 mm (1 in.) in diameter. For a typical "run," the mill was loaded with a fresh charge of ore and operated for periods ranging from 10-60 min. During this time, the current was measured with a Keithley 417 picoammeter and a chart recorder. At the end of the grinding period, the charge was removed and sieved to recover the 425, 300, and 212 µm (40, 50, and 70 mesh) fractions which were then drained and weighed. A fresh charge was used for each test and every attempt was made to keep the draining and weighing processes uniform.

Jan 1, 1985

By F. B. Foley

With the possible exception of high-speed tool steel, the service demanded of rock-drill steel is probably more precarious than that of any other tool steel. Unaided by the helpful influence of alloys and dependent solely on the efficiency of the heat treatment applied for its ability to stand up under the abuse to which it is necessarily subjected, rock-drill steel is worthy of intensive study. For its heat treatment the smith has his fire, an oil fire perhaps, and a quenching bath; he judges the temperature by his eye. There are shops where excellent drills are produced by this method, but there are more where the product varies between very good and very bad. Pyrometers with specially designed equipment are used in but few cases. But the responsibility for rock-drill failures does not rest entirely on the smith. Little has been published concerning the efficiency of drill steel, though the Canadian Mining Journal1 published the breakage record of a large number of hollow drill steels. This record indicates that most of the breaks occur during the early life of the steel and that as a given batch of steel is used, its percentage of breakage decreases. This fact, the article points out, is at variance with the much-talked-of theory concerning failure from crystallization and fatigue. It seems to point to the fact that the greater part of drill-steel failure from breakage is traceable to faulty manufacture, resulting in defects in the bore of the hollow steel from inclusions of slag or oxides, etc. As this defective material meets with early failure, it is weeded out. In addition, some breakage may be caused by a lack of proper condition with respect to heat treatment of the steel as furnished by the manufacturer. In the article mentioned, the breakage of 1/14-in (3.17 cm.) hollow steel is given as 4.62 per cent. for the early period of use, with a decrease to 3.35 per cent. and 2.67 per cent. with time in use. For 1-in. (2.5 cm.) hexagonal hollow steel, the figures for breakage are 0.18 per cent. and 0.06 per cent.; attention is called to the great decrease in breakage by the use of smaller diameter drills. The figures are given as so many drills sharpened, but there is no way of determining the percentage of

Jan 1, 1922

By T. C. Desollar

The group of iron-ore mines known as the Red Ore Mines, owned and operated by the Woodward Iron Co., is on Red Mountain approximately ten miles southwest of Birmingham, Ala. At the present time NO. 1 and No. 3 mines are active, No. 2 mines having been abandoned in 1928. Ore from this group of mines was first mined in 1882, and originally came from open cuts along the outcrop, but, when the "soft ore" (weathered hematite) was mined out and the harder ore was encountered, it became necessary to develop the orebody by means of slopes driven in the ore formation. The three mines to date have produced more than 22,000,000 tons, and the two operating mines now have a capacity of over 1,000,000 tons per year. Geology The U. S. Geological Survey has described the features of the district. It places the hematite of Red Mountain, commonly called "red ore," in the Clinton formation of the Silurian system. This formation varies from 200 to 300 ft. in thickness, and is composed largely of shale (slate) and sandstone. There are four iron orebeds in the formation, known as the Hickory Nut, Ida, Big Seam and the Irondale seams. The strike of the orebeds is northeast and southwest, and the dip is southeast, the outcrops being on the west side of the mountain. The two seams that have been worked at the Red Ore mines are the Big Seam and the Ida. The Big Seam, which is and has been the principal source of the ore mined, is approximately 20 ft. thick and consists of hematite and ferruginous bands of sandstone. It is separated into "upper" and "lower bench" ore by a slate parting that is about 30 in. thick. All present mining is confined to the "upper bench" ore, which is uniform in texture and drills and breaks fairly easily when the holes are placed so as to take full advantage of the face of the ore. Typical analyses are shown in Table 1. The presence of two water-bearing formations, the Fort Payne chert and the Hartselle sandstone, lying respectively 160 and 300 ft. above the Big Seam, make it essential that in mining the ore any movement of

Jan 1, 1934

By J. J. Gilman, T. A. Read

FOLLOWING the deformation 01 zinc monocrys-tals, sharply bent basal planes are observed near several types of inhomogeneities. Three of these in-homogeneities have characteristics which are quite regular so that they can be studied and analyzed. These are compressive kink bands, "deformation bands," and the inhomogeneities near end restraints. The present paper describes experiments in which "deformation bands" were artificially produced, and bend plane phenomena are discussed in terms of dislocation theory. Also, two new bend plane phenomena are described. The importance of bend plane phenomena in the deformation of crystals is not widely recognized. Many phenomena may be explained in a manner similar to the discussion in this paper. Jillson1 has pointed out that the "punching effect" in zinc is a bend plane phenomenon and is not caused by prismatic slip.' Bowles3 has suggested that they may be involved in diffusionless phase changes. Cahn4 has discussed the role of bend plane formation in the polygonization of zinc. Experimental Work Tensile Kink Bands: Because of the geometrical similarity between "deformation bands" and "kink bands" (compare Fig. 1 of this paper with Fig. 1 of the paper by Hess and Barrett"), the band shown in Fig. 1 of this paper will be called a "tensile kink band," and that shown by Hess and Barrett will be called a "compressive kink band." It is felt that the term "deformation band" should be reserved for banded structures in polycrystalline materials such as iron." Tensile kink bands seem to form spontaneously in aluminum crystals deformed by tensile loading.7-10 In zinc and cadmium crystals they do not form in good, carefully loaded specimens.'." However, tensile kink bands can be produced artificially in zinc crystals. The present authors did this by scratching one of the flat surfaces of triangular crystals transversely with a sharp needle. Natural tensile kink bands caused by inhomogeneities sometimes appeared in deformed crystals which were identical in appearance with the artificially produced ones. Zinc monocrystals were grown by the Bridgman method in graphite molds. Chemically pure zinc (99.999+ pct Zn) was used and the molds were sealed inside evacuated pyrex tubes during growth. The crystal cross sections were equilateral triangles with a typical base of 0.210 in. The artificial kink band shown in Fig. 1 is typical of tensile kink bands in zinc. The band lies between two bend planes which run from upper right to lower left and is inclined oppositely to the slip bands which are sharply bent at the two bend planes. The general form of the artificial tensile kink bands was independent of the scratch depth (1 to 5 mils deep) and also independent of which side was scratched. These variables did cause variations, however. Deep scratches produced more localized kink bands than light scratches. Also, if the angle between the slip plane traces and a transverse scratch varied appreciably among the three sides, then localization of the resulting kink bands also varied. Furthermore, if the slip direction lay nearly parallel to the scratched side, the band was more developed near the scratched side than at the opposite edge. Scratches produced tensile kink bands for crystal orientations from xo = 15" to x, = 75". Fig. 2 shows a scratched crystal after deformation. One triangular side lies in the plane of the photograph. The right hand tensile kink band was produced by a transverse scratch on the upper right side. The next two kink bands were the result of scratches on the front surface. The kink band at the left was caused by a scratch on the lower back side. All four bands have the same general form. A longitudinal scratch was also made on the crystal shown in Fig. 2 to determine the effect of a scratch on the critical shear stress. The critical shear stress of the scratched region was 33.9 g per sq mm compared to 24.4 g per sq mm for the un-scratched region above it. Fig. 3 shows Laue patterns of the crystal shown in Fig. 2. Fig. 3a shows the pattern of the undeformed crystal. The orientation was x, = 21°, A, = 31". After deformation, Fig. 3b was made of the homogeneously deformed portion of the crystal. The spots are compact but split into two halves. This region was elongated 45 pct and its orientation was x = 14", X = 20"; the sine law predicts x = 14", A = 20.5". Fig. 3c was taken near the center of the middle tensile kink band of Fig. 2. The pattern shows a range of orientations and polygonization in this region. The spread in orientation was due to the fact that the basal planes were curved (see Fig. 1) rather than flat as in the ideal case. Some may also have been the result of elastic distortions and "local curvatures." The orientation range was x = 23" to 32", A = 30" to 42". It is apparent from Fig. 3 that the material inside and outside the kink band rotated in opposite directions with respect to the tension axis during deformation. The orientation calculated from the ideal configuration of Fig. 9,

Jan 1, 1954

By Stanley C. Herold

A few hates on the occurrence and significance of mud volcanoes in Colombia may be of interest at the present time, owing to the renewed activity in geological exploration of the coastal regions bordering the Caribbean Sea. The best-known volcanoes are found a few miles from the seacoast. One is situated to the south of Puerto Colombia; the second, to the east of Cartagena near the village of Turbaco; and the third, near the village of Puerto Escondido south of the Sinu River. Others are reported in more inaccessible localities. Usually they stand 2 1/2 or 3 ft. (0.762 or 0.914 m.) above the surrounding ground at the crater, though several craters from 10 to 20 ft. -(3.04 to 6.09 m.) "apart will often build up an extensive mound at low gradient. The shallow mound may cover 1/2 or 3/4 acre (0.2 to 0.3 ha.) with an elevation of 12 or 15 ft. (3.65 or 4.57 m.) at the, center. The craters are formed of hardened blue clay; the inside diameters vary from 14 to 24 in. (35.56 to 60.96 cm.). The rim is continuous, except on one side where there is usually a cut 3 or 4 in. deep, thus allowing an overflow. The craters are filled to the' rim-cut with a thick mixture of blue clay mud and water, which is kept in agitation by escaping gas. Fig. 1 shows the bubble in the act of bursting and Fig. 2 the appearance of the surface of the viscous fluid a second or so later. The frequency of the explosions is determined by the weight of the column of fluid in the neck of the volcano, consequently, such explosions are not synchronous in a group of craters. Ordinarily, there arc two or three explosions in about 3 minutes. The supply of gas is small but steady and sufficient pressure must accumulate before the bubble can enter the column of fluid. The water is derived from the surface and enters the scdirnentary strata not far distant from the volcano. During long dry seasons, as the supply of water fails the volcano dries and geyser action ceases. The temperature of the muddy fluid is normal; the gas is dry and inflammable. - No petroleum products come with the gas. On the surface of the fluid, there is sometimes a dark brown streaky scum, which

Jan 1, 1920

By John B. Mertie

MONAZITE formerly was described as moribund, but, in the light of recent developments, it is no longer so. It is the common source of the rare earths and thorium, both of which are becoming progressively important in industrial and other applications. Moreover, by the action of foreign governments, the sources on which the United States has depended for its supply are now either restricted or cut off entirely. Monazite has thus become a scarce mineral and processors in this country are endeavoring to acquire it from all available sources. RARE EARTHS AND THORIUM The rare earths proper, as defined by spectroscopists, are the oxides of cerium, praseodymium, neodymium, prometheum, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutecium, with atomic numbers ranging respectively from 58 to 71. Chemists include with the rare earths scandium, yttrium, and lanthanum, with atomic numbers respectively of 21, 39, and 57. Thorium, with an atomic number of 90, is analogous to lanthanum, in that it precedes a second group of elements, whose oxides constitute the "rare earths of higher order." These are protactinium, uranium, neptunium, plutonium, americium and curium, with atomic numbers ranging respectively from 91 to 96. The last four mentioned are artificially prepared elements that so far have not been detected in nature. The rare earths with odd atomic numbers, except europium and lutecium, have no natural isotopes; and the two exceptions have only two isotopic forms. Those with even atomic numbers have from 4 to 7 natural isotopes. Samarium148 is radioactive, disintegrating over a half- life of 1.4 X 10 11 years with the emission of alpha rays. Lutecium176 is weakly radioactive, disintegrating over a half-life of 2.4 X 1010 years, with the emission of beta and gamma rays. At least 64 radioactive isotopes of the rare earths proper have been artificially prepared. Thorium is a strongly radioactive element, with a half-life of 1.39 x 1O10 years, which disintegrates through a series of 14 isotopes of 10 elements. The two longest lived and most important of these are

Jan 1, 1949

By Henry B. Smith, S. Paul Lindau

ThREe years ago it was decided by the management to granulate the matte that is produced in the smelter of the St. Joseph Lead Co. at Hereulaneum, Mo., thereby doing away with a large amount of labor in handling the matte and in subsequent crushing. On Mar. 1, 1915, the granulator was put in operation and up to Jan. 1, 1916, 18,735 tons had been granulated. The four blast furnaces have a daily output of about 280 tons of pig lead and 100 tons of matte assaying about 11.0 per cent. Pb. It is expected that projected improvements in roasting methods will eliminate more sulphur from the charge, and cut down the matte-fall to about one-half of the present figure. The blast furnaces are tapped into movable forehearths or settlers, 6 ft. by 4 ft. by 22 in., the slag overflowing into 27-cu. ft. slag cars which are hauled to the dump by electric locomotives. Previous to the adoption of granulation, the matte was tapped from the forehearths into small slag pots which were dumped after cooling. The matte cakes were broken with sledges, and transported to the crushing plant for fine crushing and screening. Here the matte was reduced to 1/4-in. size before being fed to the roaster bins. A Wedge and a Holthoff mechanical furnace are used for preroasting before sintering on the Dwight and Lloyd machines. The matte is returned to the furnaces as an iron flux until the gradually accumulating copper content reaches about 7 per cent., after which it is put aside to be concentrated in a small copper blast furnace, the resultant high-grade matte being sold. When the matte does not settle readily from the slag, two settling devices are often used, the second one being a large catch-pot, which gathers any matte that may overflow from the forehearth, the slag then overflowing from the catch-pot into the slag cars. When full of matte, the catch-pot is removed, allowed to cool, and the contents broken and crushed. a With the present plan of granulating, the matte is tapped into 6-cu. ft. iron ladles. These are transported to the granulating plant by a 5-ton

Jan 1, 1917

By R. Van A. Norris

The following tests were made, during 1889, for the Susquehanna Coal Company, to determine the relative efficiency of several styles of mine-car wheels in use at their collieries at Nanticoke, Pa. The wheels experimented upon may be divided into two classes: The "old style" (Figs. 1 and 2), which are oiled at every trip; and the "new style" (Figs. 3, 4, and 5), which require oiling about once in two to four months. Fig. 1 shows a section of a plain cast wheel, with patent annular oil-chamber. This is held in position on the axle by a square, split cotter-pin. Fig. 2 is a similar wheel, with a patent cast bushing, which is readily replaced when worn. The lubrication is effected by a simple oil-hole, but the oil is delivered a little inside of the gaugeline of the wheel, where it is most needed. Figs. 3, 4, and 5 are sections of a " new style " patented, self-oiling wheel. In this, the outer end is cast closed, and the wheel is fastened to the axle by a spring cotter-pin passed through one of the plugged holes. Dirt is prevented from entering the open end by a cap, with faced end and packing-ring, fitting over the end of the hub. The lubricant is introduced into the oil-chamber through one of the plugged holes in the hub. When the wheel is in motion, the lubricant is thrown by centrifugal force away from the axle, enters the two ports shown, and is

Jan 1, 1890

By P. H. Dudley

The present paper was suggested by the paper read by Mr. R. W. Hunt at the New York Meeting, in February last, on rail-sections (Trans., xvii., p. 778)) in the discussion of which I brought forward some of the facts and observations here stated. Professional duties having prevented me from writing out my part of that discussion in time for its publication in the volume containing Mr. Hunt's paper, I take the opportunity to present it in separate form and greater fulness. The striking features of the series of rail-sections submitted by Mr. Hunt are their shallow heads and heavy bases. In these respects they are quite similar to the section of the 80-1b. rail, which I designed in 1883 to meet the requirements of the traffic of the New York Central and Hudson River Railroad. Before the adoption of the 80-1b. rail, this road had modified its 65-1b. section from a shallow head with rounding sides and quite heavy base to one having a deep head and thin base. All the leading railroads had changed from the earlier sections of steel rails to those having deep heads and thin bases, conforming to the recommendations of the Committee on Rails of the American Society of Civil Engineers. It is but proper to say that the committee's investigations upon the wear of rails were made upon the rails manufactured under a practice quite different from that which obtained after the committee's recommendations were carried into effect. The results in actual service have been contrary to what was expected. Fig. 1 shows my 80-1b. section of 1883. Before designing this rail I had taken, at different times, a series of diagrams of the condition of tracks, with my car, on the New York Central and Hudson River Railroad, all of the New England railroads, and all but one of the trunk lines. My diagrams gave me an opportunity which could not otherwise have been obtained to see the wear of great numbers of sections of rails under widely varying conditions of traffic.

Jan 1, 1890

By R. E. J. Putman

Introduction Self-tuning regulators are a class of controllers built around the concepts of sampled data theory, and are especially suitable for implementation in a digital microprocessor or minicomputer control system. The algorithms used are distinctly different from those based upon analog control techniques and include automatic adjustment features which permit them to adapt to unmeasured changes (in, for example, ore grindability) or process nonlinearities (as exhibited by cyclone classifiers). They are also designed to handle transport lags in a simple manner, for example, anticipating the effects of a variable recycle rate on particle size distribution. The advent of distributed control systems will encourage the exploration of these techniques in the minerals processing industries, and particularly for improving the control of comminution circuits, which are especially energy intensive. This paper outlines some current work in progress on this topic. Background Those engaged in the practice of process control have long had two philosophical problems for which solutions have been actively sought - what is optimal control and how can we attain it in some heuristic fashion automatically. The basic analog controller can be represented by the differential equation: [V = Ko + K1 f y • dt + K2 dt(1)] where: v and y are the instantaneous values of output and error respectively and K0, K1, and K2 are tuning constants. The empirical rules for establishing the values of K0, K1, and K2, which provide stability, have evolved from the initial suggestions of Ziegler and Nichols(9) in 1942 and have served their purpose well. However, later analyses demonstrated that there are in fact many combinations of the values of K0, K1, and K2 which, besides being stable, behave better or worse in relation to other process control criteria; some examples are duration of error, amplitude of a damped response, magnitude or rate of movement of control valve or adjustment of speed regulator, etc. The definition of optimality had broadened. In 1964, Kalman(4) published his classic paper which tried to resolve these problems. He defined a

Jan 1, 1982

By J. S. Aronofsky

The results of polentiometric model studies and numerical computations are described. The purpose of these studies was to determine the influence of the mobility ratio on flooding efficiencies during water encroachment in petroleum reservoirs, in systems of regular well geometry. The direct line drive well pattern having relative spacing distances of one and one-half to one was investigated for water to oil mobility ratios of 10. 1. and 0.1. The results of these studies indicate that the pattern Sweep efficiency i.; very dependent upon the mobility ratio. INTRODUCTION The almost universal occurrence of water in the immediate neighborhood of oil-hearing sands lends considerable emphasis to the desirability of having a rational analysis of water encroachment into petroleum reservoirs. This problem has 1)become increasingly important with the accelerated use of water injection for secondary recovery operations. The water encroachment problem has been studied from both the theoretical and experimental viewpoints by Muskat.' He has formulated, in a precise manner, differential equations to express flow in a water encroachment system, and rigorous analytical solutions have been developed for the linear, radial, and spherical cases.' However, it becomes exceedingly difficult to solve the encroachment problem rigorously for any general two-dimensional system in which the shape of the two-fluid interface is not immediately evident from the geometry of the system. The difficulty lies in the fart that a rigorous analytical solution requires that the shape of the two-fluid interface be known simultaneously with its instantaneous posititon and with the pressure distribution on both sides of the interface. Although this paper concerns the study of the two-fluid system of oil and water. the methods described in the paper are generally applicable to other systems of incompressible and immiscible fluids in which the displacing fluid sweep-the displaced fluid down to a residual value. In each region it is assumed there is only one mobile fluid and its mobility is constant throughout the region. The Same procedure. with minor alteration, is applicable for gas injection systems provided the assumption can be made that both the displaced and displacing gases can be described by steady state formulas. For the particular two-fluid problem considered in this paper, there is a relative permeability. K, and a viscosity. p. associated with the water zone, and a different permeability and viscosity associated with the oil zone. The K/p (mobility value associated with a particular volume element of the porous medium. at any instant of time. will depend upon whether the element is ahead of. or behind the advancing interface. It is assumed that all volume elements ahead of the interface are characterized by the K/p value for oil, while all the elements behind the interface are characterized by the K/p value for water. That is. the K/p value in the oil zone is constant throughout the oil zone. and the K/p value in the water zone is also constant but different from the value in the oil zone. The symbols are defined at the end of the paper. The well pattern chosen for initial study is the direct line drive; the swept-out area at breakthrough was determined by two different methods which are described in the section on theory. These are: 1. Potentiometric analyzer 2. Numerical computation The use of the potentiometric analyzer for studying water flooding problems is adequately described in the literature, particularly for cases where the mobility in the water zone is assumed equal to the mobility in the oil zone." ' 5

Jan 1, 1952

By J. L. Thompson

There are two basic forms of the LPG-slug process: the gas driven and the water driven. The pressure required for miscibility between gas and LPG prohibits the use of the gas-driven LPG process in shallow reservoirs. The water-driven LPG slug process normally exhibits good sweep efficiency. However, displacement of the LPG by water is poor. An improvement in this process appears possible by injecting a slug of carbon dioxide between the LPG slug and the water drive. Laboratory experiments were conducted in homogeneous linear systems to determine the effect of pressure on the various displacement zones. In the carbon dioxide-LPG displacement zone, the effect of pressure on the displacement efficiency is negligible above the miscibility pressure. However, the displacement efficiency decreases linearly with decreasing pressure below the miscibility pressure. With water displacing carbon dioxide, it was found that the recovery of carbon dioxide after water breakthrough can be predicted from its solubility in water. A displacement test was conducted with LPG and carbon dioxide slugs large enough to avoid interference between the oil-LPG, LPG - carbon dioxide and carbon dioxide - water displacement zones. Under these conditions, essentially complete oil and LPG recovery was obtained. However, a substantial amount of carbon dioxide was left in the core at water breakthrough. INTRODUCTION It has been shown in homogeneous linear systems that essentially complete oil recovery can be obtained by displacement with a miscible fluid such as LPG. Economic considerations dictate that the valuable LPG also be recovered. Methods proposed for recovering the LPG include (1) displacement with natural gas at a pressure high enough to make the two fluids miscible1 (the disadvantage of this method is that the required pressure of about 1,500 psi is too high for shallow reservoirs) and (2) displacement of the LPG with water2 (principal disadvantage is that a large amount of LPG remains in the formation because of poor displacement efficiency). This paper treats an improvement in the water-driven LPG slug process3,4 where carbon dioxide is injected between the LPG and water. Carbon dioxide is completely or at least partially miscible with propane and soluble in water; thus, displacement efficiency is improved at both ends of the carbon dioxide slug. To minimize effects of other variables, all experiments were conducted in linear core systems. GENERAL PROCESS DESCRIPTION The displacements of propane by carbon dioxide and carbon dioxide by water are considered separately, assuming enough of each is injected to prevent mutual interference. Displacement descriptions are confined only to the part of the pore volume containing mobile fluids unless otherwise specified. The schematic representation is given in Fig. 1. Starting at the producing well, a zone containing only oil is followed by a zone containing a single-phase mixture of propane and oil. The concentration of propane increases in the direction of the injection well and ultimately grades to pure propane. Then follows a zone containing a mixture of propane and carbon dioxide in continuously varying proportions until 100 percent carbon dioxide is reached. In this zone, the concentration of carbon dioxide in the immobile water phase also varies from zero to full saturation. Whether the displacement of propane by carbon dioxide is of complete or partial miscibility depends on pressure and temperature (Fig. 2). If the horizontal line representing the prevailing pressure intercepts the boundary curves of the phase envelopes for the prevailing temperature (i.e., if the pressure is lower than the critical

By D. J. Jr. McAdam

Fort the past five years, an investigation of the endurance properties of metals has been in progress at the U. S. Naval Engineering Experiment Station, Annapolis, Md. As a result of the investigations at this Station1-5 and other laboratories6-11 "endurance limits" of practically all kinds of carbon and alloy steels have been determined and have been correlated with other physical properties, especially with tensile strength. About a year and a half ago, the investigation at the Naval Experiment Station was shifted to non-ferrous metals. As a result, several papers discussing the endurance properties of numerous non-ferrous metals and alloys, especially the alloys of nickel and of copper12-16 have been published. In these papers, stress-cycle graphs illustrate. the endurance properties of each individual metal and alloy, and other graphs illustrate the effect of cold working, heat treatment, and chemical composition on endurance and other physical properties. Endurance tests of non-ferrous metals were made by the machines used in the endurance tests of ferrous metals. 1-4 The specimen for the rotating-cantilever tests, which has been described, 1,2,13 has a conical surface, with taper so adjusted that the stress is nearly uniform over a length of about 1 ½ in. Alternating torsion tests were made with the machine of the inertia types17 and usually by an accelerated-fatigue method.12 As the rotating-cantilever endurance limits of metals are about twice the alternating-torsion endurance limits, the former values are more generally useful in correlating the endurance properties of nonferrous metals. In several recent papers by the writer13-16 correlation of the endurance properties of a number of non-ferrous metals has been discussed.

Jan 10, 1925

By Edwin R. Phelps, Charles W. Porterfield

BACKGROUND OF SURFACE MINING Surface mining refers to the process of removing the material (over- burden) overlying a coal seam and exposing the coal so that it can be loaded out and conveyed by trucks or other methods to the preparation plant or other facility. Surface mining has not always been important in the coal industry. In the early 1900s, almost all of the coal mined in the United States was mined by underground methods. In 1900, about 192 Mt (212 million st) of bituminous coal were mined and less than 1% was mined by surface methods. The development and use of larger equipment has allowed surface mining to gain prominence throughout the years. Table 1 shows the total production of coal by mining method in the United States for ten-year periods since 1920 and indicates the growth of surface-mined coal production. Surface mining will undoubtedly continue to account for a large percentage of the coal production in the US for many years because: 1) The capacity of surface mining excavators has continued to in- crease. Today, mining companies are using shovels (see Fig. 1) which are able to move up to 137.6 m3 (180 cu yd) in each bite and draglines (see Fig. 2) which move up to 168.2 m3 (220 cu yd) in each bucketful. 2) Increasing tonnage from the thick western coal seams is being produced by surface mining methods. 3) Surface mining has normally had lower costs and a better safety record than underground mining. 4) Surface mining normally recovers a much higher percentage of the coal reserve than can be recovered by underground mining. 5) Some coal measures can best be extracted by surface mining

Jan 1, 1981

By A. J. Phillips, C. G. Grant, Wm. B. Price

Admiralty nickel is a new corrosion-resisting and heat-resisting white metal alloy composed of 70 per cent. copper, 29 per cent. nickel and 1 per cent. tin. It has been given the trade name "Adnic." In 1924, Wm. B. Price' described this alloy and its successful use as a diaphragm metal. The physical properties of Adnic at ordinary and elevated temperatures were given in Mining & Metallury.~ A patent3 was granted on Adnic, April 28, 1925. Work was first started on this alloy during December, 1921. An investigation of the patent situation in this country and abroad, and also a search of the literature, did not reveal any work on the ternary diagram, copper-nickel-tin; and the only wrought copper-nickel-tin alloy found was that known as "Newloy," composed of copper, 64 per cent.; nickel, 35 per cent.; tin, 1 per cent. This was being manufactured and sold by Wm. Gallimorr & Sons, Ltd., Sheffield, England, for unplated spoon and fork stock, and first came to our attention in January, 1922. The preliminary work in connection with the development of Adnic was started by casting four binary copper-nickel alloys of the compositions shown in Table 1. Various a~ilounts of tin were added to each of these mixtures, to produce the series of ternary copper-nickel-tin alloys also given in Table 1. A 200-gm. sample of each of these was cast by iiielting in a clay graphite crucible and allowing the melt to slowly cool with the furnace. A longitudinal section from each of thcsc castings was polished and etched for examination. The castings were not homogenrous solid solutions, but showed the usual cored structure associated with cast alloys. Howcvrr, frorn an exarrlination of these sections we roughly determined