Search Documents

By M. J. Marcinkowski, R. M. Fisher

The flow stress-grain size relationship has been determined at room temperature in both a disordered and a fully ordered FeCo for plastic strains up to 30 pct. The results are in agreement with a Hall-Petch relation of the type given by Of =a,+kd-1/2 where of is the flour stress and a, increases mono-tonically with increasing strain to a maximum value which is much higher for the ordered than for the disordered alloy. The slope, k, is found to increase FOLLOWING the original work of Halll and petch relating the effect of grain size to the lower yield stress of iron and steel, it has been generally found that the yield stress oy.s. of polycrystalline metals with strain to a maximum and then decrease for both ordered and disordered alloys. However, k for the ordered alloy is in general higher than that for the disordered alloy and the critical strain for k max somewhat larger. All of these observations can be satisfactorily accounted for quantitatively and in some cases semiquantitatively by using a slip band-grain boundary intersection model, and by taking note of the fact that, in general, moss slip, while quite common in the disordered alloy, is extremely difficult in the ordered alloy. obeys a relation of the form oy.s.=a0+kd-1/2 [1] where a, and k are constants and d is the mean grain diameter. For convenience, and in accord with prevailing custom, Eq. [I] will be referred to simply as the Petch relation. Tjerkstra3 and Armstrong, Codd, Douthwaite, and petch4 showed that the flow stress af of iron or steel measured at strains of up to at least 20 pct also obeyed a relationship of the type given by Eq. (11. The latter investigators have also shown that Eq. [I] applies to fcc and hcp metals and alloys.

Jan 1, 1965

This report presents the comments of members of the Institute's Sub-committee on Physics of Mine Ventilation on the proposals of a special committee of the Institute of Mining Engineers (London). This report is as follows: THEORY OF MINE VENTILATION Abstract of a report submitted June 16, 1925, to the Council of The Institution of Mining Engineers by a Special Committee Laws of Flow of Aib The law of flow of air in mine galleries is, at present, expressed by two formulas differing slightly in shape but both derived from the original hydraulic formulas of Chezy and others. These formulas are: The Atlcinson Formula.—Pa = KsV2, which in transformation becomes a3 where P = pressure producing flow; K = coefficient of friction; s = surface of the mine galleries; V = velocity of flow; Q = rate of flow; a = area of mine galleries. This formula is especially applicable to mine galleries, but is unwieldy in application, as in many problems we are dealing with changes produced in the same set of airways when K, s, and a are assumed not to change, and the only variables are P and Q. Great uncertainty prevails as to the exact values to be assigned to the coefficient K in different types of airway, as different workers have given widely differing values. This formula assumes: (I) That resistance to flow is independent of the pressure within the gallery. (2) That changes in volume within the limits of pressure ordinarily met with may be neglected. (3) That changes in density and viscosity and mode of flow of the air may be neglected. (4) That the coefficient K is a constant. (5) That P is proportional to the square of the velocity. We cannot find any reliable experimental work leading us to conclude how far these assumptions are justifiable in mining practice. Equivalent Orifice Formula.—The fundamental form of this formula is Q = ~nA.\/2~11

Jan 1, 1927

By N. A. Stockett

Southeast Missouri is the largest and oldest lead-producing district in the United States. For the year 1941, the statistical picture of pig-lead production, stated in short tons (partly estimated by the Engineering and Mining Journal) is as follows. Tons World production................. 2,000,000 United States Production .........- 460,000 Southeast Missouri production..... 142,000 The consumption of primary lead in the United States in 1941 was approximately 900,000 tons, or almost double the country's production. The largest previous year's in in the United States was 718,000 tons, in 1926. The largest quantities of lead are used for cable sheathing, storage batteries and white lead. During 1941 tetraethyl lead for auto and aviation gasoline consumed 50,000 tons of lead. The entire lead production of Southeast Missouri is now mined by the St. Joseph Lead Co., whose dominant position as the largest producer in the United States of lead directly from ores is best shown by the fact that in 1941 it produced approximately 31 per cent of the lead production of the United States from its mines in southeast Missouri, where 22,000 tons of ore, averaging over 3.00 per cent lead, is mined per working day. It is known that lead was mined at Mine La Motte, Madison County, Missouri, by Renault in 1723. Other white men and Indians probably did some mining prior to that time. Since 1865, the recorded production to Jan. I, 1942, shows that the St. Joseph Lead Co. and the various other companies that have operated in St. Francois County mined lead ore, which, after milling and smelting losses produced 5,980,000 short tons of pig lead. • About 95 per cent of the present lead production of Southeast Missouri is mined in St. Francois County. The northern part of this area is 60 miles south of st. Louis. The remainder of the lead is obtained at Mine La Motte, about 25 miles southeast from the center of the producing area in st.Francois county, Prospecting In this district, most of the ore is discovered by surface and underground diamond drills and by prospect drilling underground with rock drills. Each 2-ft. length of the cuttings from these Jack-hamer prospect holes is assayed for lead. These holes are marked and the records are entered on maps. It has been found that close drilling—100-ft. centers of holes, and sometimes less—is necessary in order to locate most of the smaller commercial ore bodies, many of which previously had been missed by drilling the areas with holes spaced 200-ft. centers or more. To date, geophysical and other methods of prospecting, apart from diamond and Mining Practices of the St. Joseph Lead Company in Southeast Missouri

Jan 1, 1943

By N. A. Stockett

Southeast Missouri is the largest and oldest lead-producing district in the United States. For the year 1941, the statistical picture of pig-lead production, stated in short tons (partly estimated by the Engineering and Mining Journal) is as follows. Tons World production................. 2,000,000 United States Production .........- 460,000 Southeast Missouri production..... 142,000 The consumption of primary lead in the United States in 1941 was approximately 900,000 tons, or almost double the country's production. The largest previous year's in in the United States was 718,000 tons, in 1926. The largest quantities of lead are used for cable sheathing, storage batteries and white lead. During 1941 tetraethyl lead for auto and aviation gasoline consumed 50,000 tons of lead. The entire lead production of Southeast Missouri is now mined by the St. Joseph Lead Co., whose dominant position as the largest producer in the United States of lead directly from ores is best shown by the fact that in 1941 it produced approximately 31 per cent of the lead production of the United States from its mines in southeast Missouri, where 22,000 tons of ore, averaging over 3.00 per cent lead, is mined per working day. It is known that lead was mined at Mine La Motte, Madison County, Missouri, by Renault in 1723. Other white men and Indians probably did some mining prior to that time. Since 1865, the recorded production to Jan. I, 1942, shows that the St. Joseph Lead Co. and the various other companies that have operated in St. Francois County mined lead ore, which, after milling and smelting losses produced 5,980,000 short tons of pig lead. • About 95 per cent of the present lead production of Southeast Missouri is mined in St. Francois County. The northern part of this area is 60 miles south of st. Louis. The remainder of the lead is obtained at Mine La Motte, about 25 miles southeast from the center of the producing area in st.Francois county, Prospecting In this district, most of the ore is discovered by surface and underground diamond drills and by prospect drilling underground with rock drills. Each 2-ft. length of the cuttings from these Jack-hamer prospect holes is assayed for lead. These holes are marked and the records are entered on maps. It has been found that close drilling—100-ft. centers of holes, and sometimes less—is necessary in order to locate most of the smaller commercial ore bodies, many of which previously had been missed by drilling the areas with holes spaced 200-ft. centers or more. To date, geophysical and other methods of prospecting, apart from diamond and Mining Practices of the St. Joseph Lead Company in Southeast Missouri

Jan 1, 1943

By Perry Olcott

The Texas Gulf Coast had a rather disappointing year in the type of oil fields found. Although 17 fields were found in the area during the year, as against 21 fields in 1938, no field of major proportion was discovered. Of these 17 fields, 11 were oil fields, 4 were gas and distillate fields, and 2 were gas fields. The wildcat activity for the year resulted in about 400 dry holes, although probably 10 per cent of these were edge wells close to proved areas. During the year, 1455 oil and gas wells were completed as compared to 1637 wells in 1938, a decrease of 11 per cent. Production for the Texas Gulf Coast area for the year was 100,253,937 bbl. as against 92,530,467 bbl. produced in 1938, an increase of 8 per cent. The daily average production was 274,668 bbl. for the 365 days in the year, although only 252 producing days were allowed by the Railroad Commission; that is, 69 per cent of the time as compared to 71 days shut in for 80 per cent of the time producing in 1938. The total number of oil and distillate wells producing at the end of 1939 was 9495 as against 8451 at the end of 1938—an increase of 1044 wells, or 12 per cent. Of these wells, 6547 were flowing and 2948 pumping, or 69 per cent flowing. At the end of the previous year, 66 per cent of the wells were flowing. New Fields Angleton, Brazoria County.—The Angleton field was discovered by the completion of Glen McCarthy's No. 1 Carr in October for an initial production of 180 bbl. a day of 50" gravity oil through 11/64-in. choke with 3400 Ib. on tubing. The field is 1½ miles east of the town of Anchor. The discovery undoubtedly can be credited to the reflection seismograph, since several companies worked the area from 1933 onward with this type of exploration. The principal block was taken by the Humble company in 1934. Two deep holes by Humble revealed the presence of structure, although both were dry. The Humble and Sun companies later contributed money and acreage toward the drilling of the discovery well. The production is from a sand in the Frio, about 1700 ft.

Jan 1, 1940

By Perry Olcott

The Texas Gulf Coast had a rather disappointing year in the type of oil fields found. Although 17 fields were found in the area during the year, as against 21 fields in 1938, no field of major proportion was discovered. Of these 17 fields, 11 were oil fields, 4 were gas and distillate fields, and 2 were gas fields. The wildcat activity for the year resulted in about 400 dry holes, although probably 10 per cent of these were edge wells close to proved areas. During the year, 1455 oil and gas wells were completed as compared to 1637 wells in 1938, a decrease of 11 per cent. Production for the Texas Gulf Coast area for the year was 100,253,937 bbl. as against 92,530,467 bbl. produced in 1938, an increase of 8 per cent. The daily average production was 274,668 bbl. for the 365 days in the year, although only 252 producing days were allowed by the Railroad Commission; that is, 69 per cent of the time as compared to 71 days shut in for 80 per cent of the time producing in 1938. The total number of oil and distillate wells producing at the end of 1939 was 9495 as against 8451 at the end of 1938—an increase of 1044 wells, or 12 per cent. Of these wells, 6547 were flowing and 2948 pumping, or 69 per cent flowing. At the end of the previous year, 66 per cent of the wells were flowing. New Fields Angleton, Brazoria County.—The Angleton field was discovered by the completion of Glen McCarthy's No. 1 Carr in October for an initial production of 180 bbl. a day of 50" gravity oil through 11/64-in. choke with 3400 Ib. on tubing. The field is 1½ miles east of the town of Anchor. The discovery undoubtedly can be credited to the reflection seismograph, since several companies worked the area from 1933 onward with this type of exploration. The principal block was taken by the Humble company in 1934. Two deep holes by Humble revealed the presence of structure, although both were dry. The Humble and Sun companies later contributed money and acreage toward the drilling of the discovery well. The production is from a sand in the Frio, about 1700 ft.

Jan 1, 1940

By R. W. Smith, T. J. Smolik

Recent work indicates that fluosilicate ions and or fluosilicate amine complex ions play important roles in fluoride activation of bery and feldspars in cationic flotation systems. In an attempt to further confirm conclusions reached in this earlier work, an infrared and X-ray diffraction study of the action of fluorides in cationic flotation of silicates was undertaken. It should be noted that in recent years considerable use has been made of infrared spectroscopy in studies of surface phenomena,2-4 and these studies have established the excellence of the technique. In the present study infrared spectra were obtained for various products of the reaction of HF and dode-cyclamine hydrochloride with quartz, microcline and beryl. These spectra were compared with one another and spectra of several inorganic and organic substances. In addition to infrared spectra, X-ray diffraction patterns were run on many of the reaction products obtained. A model 137 B Perkin Elmer Infracord double beam spectrophotometer containing sodium chloride optics was used to obtain the spectra. Infrared samples, except for the dodecylamine sample, were prepared by thoroughly mixing the substance to be analyzed with purified KBr in steel vessels on a Wig-L-Bug amalgamator. One-half in. pellets weighing 100 mg were than pressed under vacuum. Details concerning percentage of the substance to be analyzed in the pellets are indicated on the spectra. In all cases except for dodecylamine a KBr pellet was placed in the reference beam of the spectrophotometer to cancel bands due to possible impurities in the KBr. The dodecylamine sample on which an infrared spectrum was obtained was prepared by placing pure dodecylamine between two salt plates. X-ray diffraction patterns were obtained with a Norelco instrument, using a copper target tube, nickel filter and Geiger tube detector. The samples were ground into powders and either placed on glass slides with glue or placed into regular powder sample holders for diffraction studies. Goniometer scanning speed varied from 1°/min to 1/8°/min. EXPERIMENTAL RESULTS AND DISCUSSION Infrared spectra of microcline, beryl and quartz were obtained first and are shown in Fig. 1. These spectra agree reasonably well with previously reported spectra.5,6 The microcline (Fig. 1 a) and beryl (Fig. 1 b) were from good Black Hills crystals. The quartz (Fig. 1 c) was from a large, clear Brazilian crystal. It is not clear whether absorption bands of minerals are due to molecular vibrations, lattice vibrations or both. Fig. 2 shows infrared spectra of dodecylamine (Fig. 2 a) and dodecylamine hydrochloride (Fig. 2 b). The dodecylamine spectrum checks quite closely with that reported in Sadtler.8 Little is known of the spectra of hydrochloride salts of amines,9 and a spectrum of dodecylamine hydrochloride could not be

Jan 1, 1965

By J. B. Newkirk, A. H. Geisler

INTRODUCTION CERTAIN of the permanent magnet alloys provide ideal systems for the study of the kinetics of the precipitation reaction and the correlation of structure with properties. One such system, Cu-Ni-Fe, was found by Bradley1,2 to exhibit a coherent transition state in the precipitation process analogous to that reported for Al-Cu alloys somewhat earlier.3 The attractiveness of some permanent magnet alloys for study lies in the fact that vertical sections of the ternary phase diagram in certain regions of composition (Fig I) have as their prototype the binary Ni-Au diagram. Alloys of this type decompose into products that have the same crystal lattice type but only slightly different lattice parameters. The advantages that such alloy systems offer for study over the usual in which an intermetallic compound is formed are many: I. Since the precipitate has the same crystal structure as the matrix, complex atomic movements are not required to form the new lattice. 2. Similarly, complex orientation relationships are not involved for both the matrix and the precipitate would be expected to have the same orientation. 3. Small disregistry of the decomposition products at equilibrium (in contrast with Cu-Ag alloys) is conducive to extensive coherent growth in the transient state and thus the transition lattice can be detected by the usual X ray diffraction methods. 4. Finally, the relative quantities of precipitate and depleted matrix can be varied from o to 100 pct* thus permitting wide freedom for the study of the effect of composition on coherent growth and properties. In the Cu-Ni-Fe alloys of appropriate composition, the face-centered cubic precipitate and also the depleted matrix when first formed are coherent with the parent matrix.1,2 The two have the same [ao] parameter as the original matrix but they are both tetragonal; the precipitate has an axial ratio c/a < I while that of the depleted matrix is c/a > I. When coherency is lost they assume the normal face-centered cubic structure with the depleted matrix having a lattice parameter greater than the original matrix and that of the precipitate less. Such a mechanism would also be expected for Cu-Ni-Co alloys because of the similarity in constitution but this had not been demonstrated. The present investigation was conducted on a Cu-Ni-Co alloy. The constitution diagram and magnetic properties of these alloys have been fairly well established 4,5 however, no previous determinations of mechanism of precipitation and no correlation of structure with properties had been made. Thus, an alloy of this system was chosen for a comprehensive investiga-

Jan 1, 1948

By R. W. Regehr, R. A. Burmeister

Epitaxial growth of GaAs 1-xPx on germanium substrates was achieved using an open tube vapor transport system. The compositional range of 0.3 < x < 0.4 was examined. The best results were obtained with (311) orientation of the germanium substrate. The physical and chemical properties of the resulting layers were investigated using several techniques. Spectrographic analyses of the layers indicate substantial incorporation of germanium into the GaAs t-X Px layer. Evidence is presented which indicates that this incorporation occurs via a vapor phase transport process rather than by solid phase dijfu-sion. Electrical measurements suggest that the germanium thus incorporated behaves predominantly as a deep donor in the compositional range of 0.33 < x * 0.40 and has a deleterious effect upon the luminescent properties of GaAs1-x Px. The increasing technological importance of GaAs1-xPx for use in light-emitting devices has led to an evaluation of several aspects of existing growth processes. The method most commonly used to prepare GaAs1-xPx for electroluminescent device applications is vapor phase epitaxial growth on GaAs substrates.&apos;-4 In a typical electroluminescent diode structure the active region of the diode is entirely within the epitaxial layer and thus the electrical properties of the substrate are relatively unimportant since it is effectively a simple series resistance (assuming hetero-junction effects to be negligible). The use of germanium rather than GaAs as the substrate material is of interest for several reasons. First, GaAs of reasonable structural quality has been epitaxially grown on germanium4-2 and it is reasonable to expect that GaAs1-xPx could subsequently be deposited on the GaAs layer. Second, germanium substrates are readily available with both lower dislocation densities and larger areas than GaAs. Finally, single crystals of germanium are more economical than GaAs single crystals. The principal objective of the present investigation was to test the feasibility of growing GaAs1-xPx epi-taxially on germanium substrates, and to evaluate the properties of such layers with regard to electroluminescent device requirements. The approach used was to a) demonstrate epitaxial growth of GaAs1-xPx on germanium, and b) characterize the relevant structural, electrical, and optical properties of the GaAs1-xPx layers. The possibility of germanium incorporation into the grown layers was of special interest since there was some indication of this in previous studies of GaAs growth on germanium.5&apos;11,12 Although a study of the electrical properties of germanium in GaAs1-xPx was not an intent of this investigation, several features of the electrical properties of the layers grown in the present study which appear to be due to germanium are described. EXPERIMENTAL PROCEDURE The open-tube vapor transport system used for the epitaxial growth of GaAs1-xPx is illustrated in Fig. 1. This system utilizes the GaC1-GaC13 transport reaction and is similar in most respects to the larger system described elsewhere.&apos; The germanium substrates were n-type, with a resistivity of 40 ohm-cm (Eagle-Picher Co.). These were cut to the orientations of {100), {111), and (3111, and were mechanically polished and chemically etched in CP-4 (5 min at 0°C) prior to growth. In some cases, a GaAs substrate was employed in addition to the germanium. The orientation of the latter was {loo}, and they were also mechanically polished and chemically etched prior to growth. The initial composition of the deposited layer was pure GaAs. After approximately 10 microns of GaAs was deposited on the germanium substrate, the phosphorus content of the layer was gradually increased over a distance of approximately 15 microns to the desired concentration and maintained at this value throughout the remainder of the growth. Typical operating parameters used during growth are given in Table I. Selenium was used as a n-type dopant in several runs to facilitate comparison of the electrical properties of the layers grown on germanium with those of layers grown on GaAs substrates, which are usually doped with selenium. The concentration of H2Se in the gas phase was adjusted to a value which would normally yield a carrier density of 1 to 5 x 101 7 at room temperature in layers grown on GaAs substrates. The terminal surfaces of the epitaxial layers were examined by optical microscopy for structural characteristics. Laue back-reflection photographs (Cu radi-ation) were also made on the terminal surface to verify the epitaxial nature of the deposit. After these steps

Jan 1, 1970

By D. L. H. Forbes

The application of the cyanide process to complex sulphide ores for the extraction of the gold and silver is no longer a novelty; but, as an example showing modern teudencies in this direction, the following description of the new milling process at the Lucky-Tiger mine is offered: The extraordinary richuess of the ore in the upper workings of this mine made any thought of milling in its early days seem unnecessary. Its location in an almost inaccessible part of the rugged mountains just south of the Arizona boundary-line, and 60 miles from the town of Douglas, made the expense of bringing in machinery and sopplies a very serious consideration. But, after the property had been shipping high-grade ore on mule-back for a few years, there remained in the mine a considerable tonnage of vein-matter that mas too low in value to ship, but which it wag thought could be milled near the mine at a profit. The first milling-experiment consisted in the installation of Nissen stamps in conjunction with concentrating-tables and Frue vanners, but, as the ore from the upper workings contained most of its silver in the form of cerargyrite, this type of mill mas not successful. The proximity of the mine to the great copper-concentrating mills of Cananea and Moctezuma naturally made the influence of copper-milling ideas felt in the company&apos;s next instdlation. At considerable expense a stage-crushing concentrating-mill, with a capacity of 100 tons per day, was built. This mill was modeled along the lines of the most approved practice in copper-concentrators at that time, the main idea being that crushing by stages .in rolls was necessary in order to prevent losses from " sliming." Largely owing to the fact that, when the mill

Jan 1, 1913

By E. C. Robertson

Observations of faults in mines, at outcrops, and in the laboratory lead to the conclusion that the displacement d of a fault increases irregularly but monotonically with the thickness t of its associated fault gouge and breccia, not including adjacent undisplaced jointed rock. The general trend of data points has a slope d/t of about 100. (The correlation coefficient of a logarithmic regression line is r = 0.94.) The rather wide scatter of the points can be accounted for by inaccuracies in measurement of d and t, and by variation in the conditions at faulting of confining pressure, rock type, water pressure, and deformation history. Limestone is an exception to the relation. Until the data can be corrected and refined, the relation should be used only qualitatively for estimating displacement of ore bodies in mines. The suggested relation is based on observations of 48 steeply- dipping normal and reverse faults and nine small flat-dipping thrust faults, with displacement less than 5 km (3 miles). It does not apply to large strike-slip and low-angle overthrust faults because their large displacements are poorly determined and their breccia thicknesses are widely variable.

Jan 1, 1984

J. H. HEGINBOTHAM, a, metallurgist of the General Engineering Co., talked on "Current Milling Practice at Kirkland Lake," at the December meeting of the Utah Section. The ore is enough alike through the whole district so that some generalizations and comparisons may be made. The question as to whether or not the flotation process should be used in the flowsheet for extracting gold by cyanide solutions is still being vigorously debated, and it will seemingly need some years for a definite answer to be given. Most of the gold is either free, though much of it is finely dispersed in quartz, or occurs with pyrite. At times there may be 2 per cent of telluride compounds in the ore, but the amount of gold telluride present is small and has not been definitely established. It has been shown by Dr. Haultain and others that though gold tellurides may be so finely disseminated that it is necessary to grind the ore exceedingly fine, the compounds themselves are not difficultly soluble. (An increase in temperature helps to dissolve tellurides, and also to settle pulps.) It is likely that if the ore were ground through 400 mesh, practically all of the gold would be soluble. As it is, with 96 to 98 per cent of the ore ground to minus 200 mesh, and some 70 per cent minus 325, the cost of

Jan 1, 1934

By E. Hein, R. A. Dodd

The fatigue softening of prior strain-hardened poly crystalline copper has been determined by measuring changes inflow stress resulting from fatigue treatments. Tensile fatigue does not soften the metal, while the softening due to reversed stress fatigue depends on the extent to which fully reversed stressing is approached. True tensile fatigue is shown to be possible only in the case of long wire specimens. Annealing following fatiguing of strain-hardened metal shows that tensile fatigue is very effective in modifying normal recovery and recrys-tallization. OBSERVATIONS by Ludwik and Scheu,&apos; Kenyon,&apos; Polakowski and Palchoudhuri, Kemsley, and Broom and Ham,596 have shown beyond doubt that strain-hardened metals are softened by reversed-stress fatigue. To some extent the softening might be associated with a rearrangement of dislocations, but the results of Broom and Ham5 on the temperature dependency of the fatigue hardening of annealed copper, and those of McCammon and Rosenberg7 on the partial recovery at 100&apos;C of fatigue-hardened copper suggest that point defects may be involved. Since lattice vacancies are the only species of point defect present in appreciable quantities in thermody-namic equilibrium, most attention has been accorded them in the various theories advanced to explain hardening and softening effects resulting from fatigue. Precise mechanisms remain uncertain, and while some effects may be due to single vacancies, defects arising from vacancy clusters may also contribute to the changes in properties. All types of plastic deformation result in point-defect formation, one frequently invoked formation mechanism involving the nonconservative motion of jogs formed by the intersection of, for example, mixed dislocations. But since fatigue deformation is thought to be a particularly effective way of forming point defects, additional mechanisms peculiar to fatigue must be sought. One possibility is that jogged loops contract during the unloading cycle to give rows of vacancies. A local high-vacancy concentration could conceivably promote polygonization and recovery by climb, and, therefore, could explain the fatigue softening of strain-hardened metals under appropriate conditions of temperature. Conversely, the experiments by Broom and Ham6 on the fatigue hardening of copper single crystals involving subsequent tensile testing of previously fatigued specimens, resulted in the observation of distinctly lowered yield points. This could be due to vacancy atmospheres associated with dislocations, possibly augmented by jogs on dislocations. In addition to the yield-point phenomenon, a post-yield hardening was observed, with a temperature-dependence resembling the friction-hardening of irradiated metals,9 this again suggesting a point-defect mechanism. An important development in this field has been the observation,10 by transmission electron microscopy, of high concentrations of prismatic loops in fatigued aluminum. By analogy with quenched aluminum filmso11 it seems certain that these loops originate in the collapse of vacancy clusters formed during deformation. Metals, such as copper, having a relatively low-stacking fault energy would tend to produce Frank sessile loops (in practice tetrahedral defects with stacking faults on all (111) planes) rather than the glissile prismatic loops observed in aluminum. The manner in which these various defects affect the different aspects of fatigue behavior has not yet been fully investigated. The present work was designed principally to indicate whether tensile fatigue gives rise to hardening and softening effects similar to those associated with reversed stress fatigue, and with the hope of providing additional information on the contribution of point defects to fatigue deformation. Despite the uncertain ty often associated with the interpretation of resistivity data, i.e., the relative contribution of stacking faults and other defects, such measurements are conveniently employed to study point defect pheno-

Jan 1, 1962

By R. P. Laforce, ZJ. R. Low, A. M. Turkalo, D. F. Stein

The interaction of the crlloying eletnenls, nickel and chromium, with the impurity elements, antimony, pIzosphorus, tin, and arsenic, to producse reversible temper brittleness in a series of high-purity steels containing 0.40 wt pct C has been investigated. The alloyed steels contained approximately 3.5 pcl Ni, 1.7 pct Cr, and 0.05 to 0.08 pct of the particular irnpurity to be investigated. Susceptibility to teirlper embrittlement was measured by comparing the notched-bar transition temperature of each steel after quenching from the final temper and after very slow cooling (step cooling;) following the final temper. A plain carbon steel without alloying elements, bu/ ud/h 0.08 pel Sh, does not embrittle when step-cooled through the emzbrittling range of temperatures. The same embrittling treatment, applied to a steel with about the same antinzony content but with nickel and chvonziunz added, causes a 700°C increase in transition temperature. If chromium or nickel is the only alloying element, the increase in transition temperature is only 50%, again with antimony present. A carbon-free iron containing nickel, chromium, and antimony shou~s a 200°C shift in transition temperature for the same thermal treatment. Specific alloy-impurily interactions are also observed for the other impurity elements, phosphorus, tin, and arsenic. Additional investigations involving electron microscopy, trzicrohard-ness tests of vain boundaries, minor additions of zirconiutn and the rare earth and noble metals, nzainly with negative results, are also described. HE particular type of embrittlement investigated is that which is encountered in alloy steels tempered in the temperature range from about 350" to 525&apos;C or slowly cooled through this range of temperatures when tempered above this range. This type of embrittlement is sometimes called reversible temper brittleness to distinguish it from the embrittlement indicated by a minimum in the room-temperature V -notch Charpy energy vs tempering-temperature curve encountered in the range 28 0" to 350°C. Temper brittle-ness seriously restricts the use of many alloy steels since it precludes tempering or use in the embrittling range of temperatures and may significantly raise the ductile-brittle transition temperature of heavy-section forgings and castings tempered above the embrittling range, since such sections cannot be sufficiently rapidly cooled after tempering to avoid embrittlement. The very voluminous literature of temper brittle-ness up to about 1960 has been reviewed by woodfine&apos; and LOW.&apos; Of particular significance to the present investigation was the demonstration by Balajiva, Cook, and worn3 that high-purity Ni-Cr steel does not exhibit temper brittleness and the subsequent detailed and systematic study by Steven and Balajiva~ of the effect of impurity additions on the susceptibility to embrittlement of Ni-Cr steels. Steven and Balajiva showed that, of the impurities which may be found in commercial steels, Sb, As, P, Sn, Mn, and Si could all produce temper brittleness in a high-purity Ni-Cr steel. The principal purpose of the present investigation was to study the effects of particular alloy-impurity combinations on susceptibility to temper embrittlement. The steels used were high-purity 0.30 to 0.40 wt pct C steels containing 3.5 wt pct Ni and 1.7 wt pct Cr, separately or in combination. The susceptibility of these steels was then determined when approximately 500 ppm by weight of antimony, arsenic, phosphorus, or tin were added as an impurity. The melting, casting, and forging practices used in the preparation of the materials investigated are described in Appendix A. Table A-I in this appendix shows the analysis of all steels to be discussed. The steels were produced as 20- or 2-lb heats. The smaller heats were used after it had been demonstrated (see Appendix B) that a small, round, notched test specimen could be used to measure the shift in the ductile-brittle transition temperature caused by temper brittleness with about the same result as that obtained by Charpy testing. HEAT TREATMENT Unless otherwise noted, all steels were tested for embrittlement in the tempered martensitic condition. A typical heat treatment for a 0.40 C, 3.5 Ni, 1.7 Cr steel was: 1 hr at 870"C, in argon, quench into oil at 100"C, quench into liquid nitrogen, temper 1 hr at 625"C, and water-quench. The warm oil quench was used where quench-cracking was encountered; otherwise the initial quench was into room-temperature oil or water. For other compositions austenitizing temperatures were 50°C above Acs with the remainder of the thermal cycle the same. Steels in this condition, with no further heat treatment, are designated as non-embrittled. The above quenching and tempering cycle for the 0.40 pct C steels resulted in as-quenched hardnesses of 48 to 53 RC and as-tempered hardnesses of 24 to 31 Rc except in the case of the plain nickel or plain carbon steels. In these, the as-tempered hardness was as low as 80 to 90 Rg. No attempt was made to adjust the tempering temperature to obtain the same hardness in ali steels since it was felt that a uniform thermal cycle was more important than exactly equivalent hardness values. Pro- the standard quench and temper described above, the standard embrittling treatment was "step-cooling". For this the thermal cycle was: 593"C, 1 hr; furnace-cool to 538"C, hold 15 hr; cool to 524"C, hold 24 hr; cool to 496"C, hold 48 hr; cool to 468&apos;C, hold 72

Jan 1, 1969

By J. H. Brophy

Experimental evidence in recent years shows that nickel coated hydrogen reduced tungsten powder can be sintered to 98 pct of theoretical density at 1100°C. New data indicate that the sintering rate is the same for nickel contents ranging from 0.125 wt pct (mon-atomic layer) to 5.0 wt pct Ni coated on 0.561. tungsten powder. Nickel tungsten made by coreduction from oxides sinters in a kinetically similar way, but the rate tends to increase with higher nickel contents. The activation of sintering can be accomplished with a minimum amount of nickel if coated powder is used. Transverse rmpture strength was found to increase in specimens containing 0.25 pct Ni as density increased during the initial stage of the carrier-phase sintering process. Upon the onset of grain growth in the final stage, strength was found to decrease. With increasing nickel contents up to 4 pct, strength increased. Maximum strengths in three-point loading were observed at 73,000 psi for 0.25 pct Ni and 93,000 psi for 5 pct Ni. These were comparable to that of massive tungsten recrystal-lized in the presence of nickel and tested in the same way. The results were sensitive to the mode of powder treatment and ductility was negligible in all cases. The study and application of sintered bodies of nickel and tungsten is not new; however, the analysis of the mechanism by which small additions of nickel increase the sintering rate of tungsten promises to Contribute new information regarding sintering theory in general. Initial experimental evidence was presented by the authors showing that nickel-coated hydrogen-reduced tungsten powder may be sintered to 98 pct of theoretical density at 1100°C in 16 hr.&apos; Simultaneously, a kinetic analysis of the process showed that it took place in two distinct stages. In the first stage, nickel evidently served as a carrier phase through which tungsten atoms could move. This stage was kinetically similar to the &apos;solution-precipitationo step postulated when the carrier phase is liquid3 although in the nickel tungsten case, there is no evidence of the existence of a liquid phase either in equilibrium phase relationships or in mi-crostructures at the temperatures under consideration. In the present work, new data for nickel-coated tungsten powder are offered in support of the proposed mechanism, and a more explicit study of the second stage of densification is presented. Concurrently, the sintering kinetics of these coated powders are compared to Ni-W powder made by coreduction of oxides. In this way the present work can be compared to earlier results in nickel activated sintering of tungsten in which the coreduction process was emplyed. The ultimate utility of such an activated sintering process will be determined to some extent by the mechanical and physical properties of the final prod-

Jan 1, 1962

By J. H. Henderson, L. A. Wilson, R. L. Gergins, R. J. Wygal, D. W. Reed

This paper presents a method of predicting the production history of an underground combustion recovery process. A rigorous solution of the thermodynamics and hydrodynamics involved is beyond the scope of this report. However, a practical scheme to appraise combustion recovery performance has been Worked out. By prudent assumptions, regarding the attainment of steady-state conditions, a trial-and-error solution, which satisfies both material balance and three-phase relative permeability requirements has been evolved and tested. As a combustion zone moves through a formation the interstitial water, the water of combustion and a portion of the oil wil1 be vaporized. These vapors will move downstream to a cooler region of the formation where they will condense. Part of the remaining oil will be displaced by the imposed gas drive and what remains behind will be consumed as fuel. The fluids will distribute themselves downstrean? in a manner which will satisfy the three-phase relative permeability characteristics of the formation. Three distinct zones will exist ahead of the combustion zone: (I) a zone termed a water bank which contains three mobile phases, oil, water and gas; (2) a region containing two mobile phases, oil and gas, called the oil bank; and (3) a zone having the fluid saturution distribution which existed prior to combustion. The mobile water will impose a water flood on the oil in the region containing three flowing phases. The process can be visualized as a simultaneous water .flood and combustion-supported gas drive. It is possible to estimate the saturation distributions in the water bank and oil bank as well as the production history for any combustion temperuture if the porosity, three-phase relative permeability characteristics, oil viscosity and initial saturations are known. This has been done for injection pressures ranging from I to 100 atm, oil viscosities of 10 to 1,000 cp and porosities from 20 to 40 per cent. Several of these calculations have been checked in the laboratory, with the result indicating rather good agreement between the predicted and observed production histories. The analytical and experimental techniques are described and the comparison of predicted and observed performance presented. INTRODUCTION Considerable research by the oil industry during the past 10 years has been directed toward the thermal recovery of crude oil. Of all schemes considered, the one receiving the most attention is in situ combustion. This is a process in which part of the oil is actually burned within the reservoir rock. The uniqueness of the process lies in its potential. Theoretically, this potential generates from the following: (1) it may open the door to vast reserves previously not economically producible, (2) it may induce increased production rates where low rates are now realized and (3) it may give high over-all recovery efficiency. The general idea of the process has received considerable attention in the literature &apos;-&apos; and the following brief description is intended for orientation only. In situ combustion can be visualized by considering a linear system, one end of which represents the injection well and the other the producing well. The formation at the inlet end is raised to ignition temperature by placing a gas or electric heater at the face of the formation or by the ignition of thermite, charcoal or similar material. While heating, the water and part of the oil in the heated region is vaporized and moved out into the reservoir by the injection of gas containing oxygen. In addition, part of the oil is displaced as liquid by the imposed gas drive. The oil not displaced is modified to an immobile, coke-like material (hereafter referred to as coke) by the high temperatures existing immediately ahead of the combustion zone. This coke is used as fuel, and the combustion front advances through the formation at a temperature which is probably in excess of 800°F. As the combustion front advancek it will drive ahead all interstitial oil not rendered immobile and all interstitial water plus the water formed by the combustion of hydrogen. As a result the sand behind the combustion zone is freed of all oil and water. Although the general description of the process has been outlined in the literature, there has been no consideration of the behavior of the fluids moving downstream from the combustion front. It is the purpose of this paper to present a technique

By P. R. Sahm, T. V. Pruss, D. A. Gandolfo

Cb 3 Sn powders were hot-pressed to estahlish densi-fication conditions and assess the possible use of such compacts in multiphase structures with ceramic or magnetic inclusions. Superconducting transition temperatures, Tc, were measured as a function of powder particle size, pressing temperature, and second-phase admixtures. The highest transition temperatures were found in coarse powder (5 to 500 u) compacts and were only weakly depended on pressing temperatures up to 1200°C. Fine powders (below 5 p), however, both single-phase CbsSn and Cb3 Sn-composites, showed a stronger dependence on hot-pressing temperatures. While Al2 O3 phase admixtures did not affect T, much more, a Pronounced T, degradation was observed upon the addition of ferrimagnetic Fe2 Mno. 5 Zno.5 O4 powders. Likewise, critical current densities, Jc, at 4.2° K were lowered appreciably in the ferrite doped samples, whereas the neutral A1203 inclusiow gave slightly improved Jc values. MULTIPHASE structures in electronically active materials have recently gained in interest as pointed out by Galasso in a review article.&apos; In superconductors the most widely reported group are eutectic alloys which have been mostly investigated with respect to the proximity effect.2"4 In addition, "artificial eu-tectics", for example in the form of mercury-vycor glass sponge5 or fine niobium wires imbedded in a copper matrix,= have been prepared to attain higher critical fields and critical current densities. The idea was to enhance flux pinning phenomena by second-phase inclusions or ho1es. 7 Flux pinning should also be possible by the introduction of insulator inclusions into a superconducting matrix. Ceramic-metal combinations are most easily produced by hot pressing (= pressure sintering), as it permits an almost unlimited selection of material combinations. Cb 3 Sn has been prepared by vapor phase growths or in the form of thin films. Large compacts must be sintered,1° however, and normally present difficulties. At temperatures below 1350°C insufficient densities are obtained and at higher temperatures the loss of tin due to dissociation upsets the stoichiometry. Hot pressing is a natural approach to circumvent the problems, since one can obtain satisfactory densities despite low sintering temperatures. This work was mostly concerned with establishing conditions to hot press Cb3 Sn and Cb3 Sn multiphase structures (= composites), because no data are presently available, and to evaluate these with respect to their transition temperatures. However, a few measurements on critical current densities were also carried out, in particular to assess the value of ferrimagnetic inclusions. I) EXPERIMENTAL PROCEDURE The experimental procedure involved the preparation of feed material and powders, hot pressing, and evaluation of the resulting ingots. As no attempts were made to synthesize Cb3Sn from the elements during hot pressing, feed material had to be produced. For this purpose, a stoichiometric Cb-Sn powder mixture was compacted into a 3-cm-diam ingot (80,000 psi) and then inserted into a quartz tube and evacuated. Rf heating was employed. Above the tin melting point (230°C) liquid tin was forced out of the ingot, but was pulled back by capillary action after approximately 0.5 hr of continuous pumping at 700°C. Thus, it appears that evacuation at this temperature caused desorption of impurity gas creating wetting surfaces which, later on, favored alloying at relatively low temperatures. After a presintering period of 17 hr at 800°C, the quartz tube was tipped off and sealed into another such larger-diameter tube which, in turn, was connected to a pump system. This configuration permitted a temperature treatment at 1400°C, carried out for 65 hr, without collapsing of the glass walls or unfavorable chemical interaction of Cb3Sn with the quartz. The resulting material was

Jan 1, 1969

By W. C. Ellis

IN an ingot of germanium solidified progressively from the bottom by a method&apos; devised by J. H. Scaff and H. C. Theuerer, examination discloses ex- IH. C. Torrey and C. A. Whitmer, Crystal Rectifiers. p. 364. 1948. New York. McGraw-Hill Pub. Co. tensive twin relationships. A slice taken about midway in a cylindrical ingot approximately 3/4 in. in diameter and 1 1/2 in. in length, after etching and polishing to delineate different orientations, is shown in fig. la. The orientations of the regions designated with letters were determined by Laue X-ray back-reflection methods and plotted on stereograms. The orientation relationships of the designated components were determined by comparing the values for the nine angles between the three respective cube poles of each orientation with the values calculated in a formal treatment of octahedral multiple twinning in cubic crystals. Germanium, diamond cubic in structure, has the octahedral twinning habit. I am indebted to K. H. Storks for the calculation of the angular relationships of cube poles in octahedral twinning to four orders. The set of values for the nine angles is distinctive of the order of twinning. Confirmation for a multiple twin relationship is obtained from the determined indices of the mirror planes. These exist for all orders of twinning through the third and for some of the fourth." If the orientations are not those for twinning, then the nine angles for the cube poles do not correspond in value and distribution to those formally calculated. Since all nine angles must correspond in values and distribution of values to the calculated ones, the Laue method with a precision of one or two degrees is adequate to establish or deny with confidence the existence of multiple twins. Regions of the same orientation can also frequently be identified by the optical reflections. For example, the narrow twin bands in A at 2: 00 o&apos;clock have orientation B1. The interesting twin relationships shown schematically in fig. lb were found for the section in fig. la. Most of this slice was made up of orientation, A, appearing in widely separated regions. Of the four possible first order twins of A, three were present in this slice and are designated by B with subscripts. Four second order twins of A are designated by C with subscripts. It is worth emphasizing that two of these, C, and C,, are second orders of A through the first order missing in this section. Two regions, designated by D with subscripts are third order twins of A. D2 is a sixth order twin of D,. All orientations found were ascribable to multiple twinning, as if the orientations in this section originated earlier in solidification from a single nucleus. The presence of extensive multiple twinning to- gether with the absence of other orientations appears to be a characteristic result in many instances of solidification of germanium. Fertile conditions for twinning probably exist in the array of atoms in the diamond cubic structure. The high order twins in the section shown, it is reasonable to presume, are the result of progressive octahedral twinning through several generations in the material freezing earlier. Some of these generations do not appear in this section, it is suggested, because their orientations with respect to the growth direction were unfavorable for survival. The extensive twinning is probably promoted during solidification by constraint imposed by volume increase, and to an irregular growth front. Twinning may also be due, in part, to the attempt of the solidifying region to attain the orientation most favorable to the growth direction (maximum thermal gradient). The nucleus for a twinned orientation could have its origin in a "stacking fault" on the close-packed octahedral plane. Further work is being done in which the course of twinning throughout an ingot is being studied. The results appear to be important in the general theory of solidification.

Jan 1, 1951

By R. A. Harrington

THE structure of anodic films formed on aluminum and other metals under varied conditions is not well known despite the wide use of such films both as protective coatings and as the dielectric medium in elec-trolytic condensers. The present work was undertaken as a survey of the possibilities of electron diffraction in the investigation of anodic films, especially in comparing the properties of anodic films formed under dif-ferent sets of conditions and subjected to various subsequent treatments. In addition, an effort has been made to compare surface films formed on aluminum by anodic treatment with surface films formed by heating, immersion in chemicals, etc, The electron diffraction method in many cases has been successfully applied to the study of thin surface films. Its principal advantage is that it can be used without removing the films from the base material upon which they have been formed. The low penetrating power of electrons, in the "reflection" diffraction method which has been used in this work, prevents the appearance of diffraction patterns from substances at depths greater than about 100 Angstrom units (10-6 cm.). Different investigations of the structure of anodic films have shown widely varying results, depending on the methods used in preparing the films. Apparently under some conditions these films are crystalline and under other conditions they are amorphous, and it has been difficult to say which type of structure will be found in any particular case. Schmid and Wassermann&apos;s&apos; X-ray diffraction patterns of eloxal? films show two broad, diffuse bands, which these investigators attribute to finely divided cubic y-Al2O3-§ Burgers, Claassen, and Zernicke3 obtained sharp X-ray

Jan 1, 1940

By C. F. Gates, H. J. Ramey

Recent literature shows that pronounced increases in oil recovery can result from the use of miscible systems in recovery operations. This literature also points out certain problems associated with maintaining miscibility, e.g., compositional changes resulting from alterations in pressure and temperature or from zone dilution. The purpose of the work described in this paper was to study miscible zones for possible use in waterflooding operations and examine the manner in which these zones break down. The fluid system selected for study was oil—terNary-butyl alcohol—water, which, because of its narrow range of miscibility, is ideally suited for investigation in short, linear systems. The laboratory-observed effects on oil recovery and zone stability of a number of variables are reported. Among the variables investigated were miscible zone size, viscosity ratio, length of travel, and interstitial water saturation. Results obtained with this system show that interstitial water adversely affects recoveries because of premature phase break. Salinity of the water further aggravates Ais situation. This effect, although pronounced for this system, would probably occur in any fluid system containing an alcohol. As expected, viscosity ratio has a decided influence on recovery efficiency and zone stability. The results also show that use of a suficieno zone size, even though the system has poor phase characteristics, yields higher oil recoveries than are obtained from straight water floods. Length-of-travel studies showed a square root relationship between zone growth and path length for favorable viscosity ratios. No such clear-cut dependence was observed under unfavorable viscosity conditions. INTRODUCTION As new oil reserves have become increasingly more difficult and expensive to find and develop, the oil industry has devoted more and more time and money to finding more efficient methods for exploiting known reserves. The increasing number of water floods is one manifestation of this attempt to improve oil recoveries from existing fields. Since considerable quantities of oil are by-passed by the waterflood process, it is only a partial answer to the problem. The search continues. Of late, several proposed processes have received the critical attention of investigators. Among them are gas drives, in situ thermal reactions and miscible displacements. The present paper is concerned with miscible displacements in conjunction with water floods. Recent literature1- reports that, under proper conditions, oil recoveries from LPG floods, propane sweeps, condensing gas drives, etc., approach 100 per cent of the oil in place in the region contacted by the flood. This literature also points out some of the problems associated with these processes, one of the main ones being the maintaining of miscibility. Compositional changes resulting from pressure and temperature variations or from zone dilution give rise to phase breaks and loss of miscibility, the conclusion being that, after loss of miscibility, much of the beneficial influence of the zone is lost.&apos; The results of the subject work show that, if sufficient zone material exists ahead of a phase interface, considerable improvement in oil recovery can be obtained. In order to increase our understanding of the behavior of miscible systems as they degenerate into immiscible processes, a laboratory system having rapid deterioration characteristics was needed. The fluid system oil—ter tiary-butyl alcohol (TBA)—water possesses these properties and was the system investigated. Although these fluids are different from those generally employed in miscible studies, an understanding of their behavior can be applied to other miscible slug processes. However, under conditions where mass transfer maintains a miscible system through multiple contacts, e.g., enriched gas drive or high pressure gas drive, the observed behavior of alcohol zones would not be applicable. The variables of interest were zone size, viscosity ratio, length of travel, initial water saturation, rate and core characteristics. Of these, only the effects of the following on zone breakdown and oil recovery are reported in detail: (1) zone size, (2) path length, and (3) initial water saturation. The effects of viscosity ratio and core characteristics are discussed in conjunction with other variables. Although initial water saturation is not envisioned as important to the phase behavior of hydrocarbon systems, e.g., LPG, it is important in alcohol systems. The properties of the fluids and cores used are given in Table 1. As previously stated, this fluid system was selected because of the limited range of miscibility