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By J. W. Hickman

INTRODUCTION MOST of the electron diffraction studies of oxide films which form on metals and alloys have been carried out by oxidizing the specimens in an auxiliary furnace, cooling down to room temperature and then inserting the sample in the camera and taking a diffraction photograph. Prior to the investigations at the Westinghouse Research Laboratories, no systematic study of the oxidation of any metal or alloy had been made over a wide temperature range with photographs taken at elevated temperatures except the investigation of iron by Jackson and Quarrell.1 In order to interpret the electron diffraction patterns of the oxides which may form on alloys, it seemed advisable to make a comprehensive study of the oxidation of the purest metals available in the bulk form. Thus far studies have been completed on iron,2 cobalt,2 nickel,2 chromium ,2 Copper2, tungsten,3 molybdenum,3 beryllium ,4 uranium,4 thorium4 titanium5 and zirconium5 while investigations are in progress on tantalum and columbium, The next step in the study is concerned with the investigation of the oxides which form on binary alloys. Some of the alloys consist of a single, phase while others contain more than one phase. The identification of the oxides on the surface of a binary alloy may be more difficult than on the metals since oxides containing both metals as well as those of each metal separately may form. Furthermore, it is possible that solid solutions of the various oxides may occur. In these cases the electron diffraction method may not be able to identify the oxidation products unequivocally, Examples of solid solutions which may present difficulties are MoO2 and W02, Fe3O4 and FeO-Cr2O3 since the diffraction patterns are so similar. Since electron diffraction can determine only the structure of the oxide, the chemical composition must be inferred from the diffraction data based upon X ray diffraction investigations of specimens of known composition. It is possible in some cases to decide whether a given solid phase reaction can occur on the surface of an alloy by a study of available thermodynamic data. Table I lists the equations for the formation of most of the oxides from the elements together with values of log10 KR for the several temperatures. [OF°R = -RT In KR 0 and-~75T = logi°KR] [?F°R] and KR are the free energy and equilibrium constant of the reaction. Calculations may be made using the values given in Table I to determine whether a given solid phase reaction is possible thermodynamically. For example, a solid phase reaction should occur between aluminum and chromium' oxide to form

Jan 1, 1948

By Stanley Gill

The apparatus is composed of sections of small diameter, seamless steel tubing welded into a continuous flexible tube. At the bottom end a 1/4-in. pipe nipple with a 10 to 15-lb. weight is attached, together with a registering thermometer and a pair of ball check valves. The entire length of tubing is coiled in a single layer upon a drum 4 ft. in diameter which can be attached to the platform of a truck and provided with devices for winding and unwinding the tubing. Connections are made with the upper end of the tubing through a stuffing box, thence to a gas manifold to which a pressure gage is connected. Hydrogen gas is carried in standard 2-ft. cylinders and readings are taken by admitting gas into the tubing from one (or both) of the hydrogen cylinders until the pressure has been built up above that to be measured. At this time the gas supply is cut off. Excess gas escapes through the open end of the tubing and when equilibrium is reached, the pressure is read at the surface gage. Corrections are made for the weight of the column of gas. The advantages claimed for the apparatus include accuracy and the ability to measure the pressures at any number of points without removing the gage. Among the disadvantages of the apparatus are the somewhat bulky size of the equipment and its relatively high initial cost.

Jan 1, 1933

By T. F. Witherbee

AS the forms of blown-out furnaces are of much interest to ironmasters and metallurgists, the manner of taking the accompanying sections of the Cedar Point stack is here given. The diagrams show the original and also the final shape of the furnace after a two years and twelve days' blast,, during which the following solid materials passed through it, viz.: Coal, 41,000 tons; ore, 57,000 tons; limestone, 30,000; total, 125,000 gross tons. Product, 411/4 tons per day Bessemer pig iron. The apparatus used in taking the sections was a modification of that proposed by Mr. Frank Firmstone,* and consisted of a sliding rule, to follow around the circumference of the stack, which rule was connected by a string to a segment of a circle of 24 inches radius. The segment was carried by an arm which connected it to a huh as a centre, 2 inches in diameter. A second string was wound around the hub, and communicated motion to a pencil-carrier, the pencil of which marked out on paper the exact outline, and reduced it to a scale of & inch to the foot. The whole machine was made in about three hours, with the facilities of a carpenter's shop, and gave in operation every irregularity of the lining. The sections were taken at salient points, by lowering a hanging staging on which the apparatus was placed. Tracings from the paper of the machine were made, and, as in this case several copies were required, the tracings were glued on to thin sheets of basswood, and patterns carefully sawed out with a bracket saw.

Jan 1, 1879

By A. Gittens

In two recent papers stevens13,14 has compared the methods used by various investigators to calculate the contribution of grain boundary sliding to the total creep strain. In previous work Gittins15 has shown that the strain due to grain boundary sliding Egb may be estimated from the lateral, d, and vertical, v, displacements of a longitudinal marker line as it crosses a grain boundary. He obtained the formula, where nL is the number of grains per unit length measured on the specimens before creep, and \p and ?2 are, respectively, the angle between the grain boundary and the stress axis in the plane of the surface and normal to the surface (see Ref. 13, Fig. 1). The subscript L indicates that observations are made in a longitudinal direction parallel to the stress axis. It was generally found more convenient to measure the grain size of a specimen before creep; this was necessary to characterize the specimen. Stevens13,14 however prefers to define Egb in terms of NL, the number of grains per unit length after creep. Since nL - NL(l + €1) where cr is the total strain, Eq. 1 11 becomes The quantities d and ?, can be determined directly from the marker lines, while v and ?2 are found by sectioning normal to the surface. In the interior when symmetry considerations suggest that v = d and ?1 - ?2 the strain due to grain boundary sliding may be estimated from a suitable internal longitudinal marker line by the equation To determine cgb at the surface using either Eqs. |1| or [2] requires a large number of observations, particularly if many estimates of cgb are required, and also it is impossible to determine the variation of cgh with creep strain on the same specimen because the specimen must be sectioned to determine ?2. Gittins15 found that for a number of materials the sliding vectors d and v were related to each other so that provided one was measured the other could be estimated. Also during creep, grain boundaries tend to migrate to meet the surface at angles close to 90 deg,16 so that the term nL(v/tan?2)L was comparatively small when 4,- 90 deg. By determining the frequency distributions of ?2 on control specimens this term can be estimated without sectioning the creep specimen. In this way an empirical equation based on Eqs. |1| and |2| enables cgb to be determined with reasonable accuracy with fewer observations of the angles and sliding components. For B brass, the relationship between the sliding vectors indicated that ceb = 0.85nLVL . In Table I of Stevens paper this equation is stated to be incorrectly derived. However it should be pointed out that this is an empirical equation derived from Eq. |1|, based on a knowledge of the relationship between d and v and on the frequency distributions of ?1 and ?2 for a particular material under given experimental conditions. It was used only when these relationships were known, to reduce the number of observations required to estimate cb. Therefore the comment "derivation incorrect does not apply. Gittins did in fact make use of Eqs. |1| and 131. Author's Reply I must apologize to Dr. Gittins for the inadvertent misrepresentation of his work. Other slight errors in Table I have been pointed out to me. Langdon (No. 12 Table I), Gifkins (No. 7, Table I), and possibly other workers did not measure the number of boundaries per unit length after creep (A') but the corresponding quantity bejove creep (n). As Dr. Gittins points out, a completely analogous set of equations to those given in the paper can be derived by the same method: using the number of boundaries per unit length before instead of after creep. The basic equations corresponding to Eqs. [2] and 171 of the paper, from which all the others can be derived, are

Jan 1, 1968

By S. G. Epstein

Electromigration has been measured in dilute liquid alloys of lead in antimony and antimony in lead. In these alloys antimony migrates with the electron current; lead migrates in the opposite direction. These results, which contradict the mass criterion, were predicted by the electron drag model for electromigration in liquid alloys. The existing experimental data are shown to correlate with the difference in electrical resistivities of the alloy components. FOR many years investigators have attempted to relate observed electromigration phenomena in liquid alloys to the physical properties of the alloy components. The most successful correlation was found by Angus et' al.,1 who in 1959 proposed an empirical criterion for predicting the relative direction of motion of the components of a liquid alloy in an electric field: the component with the smallest atomic mass concentrates at the cathode. While this criterion is obeyed in nearly all the alloy systems which had been investigated, the physical basis for such an effect was not understood. It was also disturbing that the mass criterion predicted the wrong sign for the Haeffner effect; observations with pure liquid metals revealed that in every instance the lighter isotope was transported to the anode.2 Klemm3 explained these isotopic separations by suggesting that the lighter isotopes were more mobile and more easily carried to the anode with the electron stream. Additionally, several deviations from the mass criterion have been found in liquid alloys, notably involving transition metals such as chromium, nickel, palladium, and zirconium, which migrate to the anode in liquid bismuth.4'5 Recently, a model has been proposed6 in which electromigration in liquid alloys is attributed primarily to the interaction between the electron stream and the metal ions. In essence, this model predicts that the component with the greater electron-ion scattering cross section will be preferentially transported to the anode, displacing the other component to the cathode. The electrical resistivity of each pure component at its melting point is taken as the measure of its scattering cross section. This model was developed from the results of systematic studies with various solutes in liquid mercury,7'8 bismuth,9 and sodium.10 In every alloy, the component with the greater resistivity has centrates at the anode. Coincidentally, in every instance the component with the greater resistivity has also the greater mass, apparently satisfying the mass criterion. In order to differentiate between electron-ion coupling and atomic mass as the relevant physical prop- erty influencing electromigration, measurements were made with Pb-Sb alloys. Lead has an atomic mass nearly twice that of antimony, but lead has an electrical resistivity of 91 microhm-cm while antimony has a value of 113.5 microhm-cm at their respective melting points. The mass criterion predicts that in an alloy of the two antimony will concentrate at the cathode; the electron drag model predicts that antimony will concentrate at the anode. EXPERIMENTAL To conclusively determine the relative motion of lead and antimony in each other, solute electromigration was measured in dilute liquid alloys of antimony in lead and lead in antimony. Both starting materials were 99.999+ pct pure. The measurements were made with the same capillary-reservoir technique previously used for measuring electromigration in liquid bismuth alloys.11 Several changes in the experimental apparatus were necessary, however, to accommodate liquid antimony, which has a higher melting point than bismuth. The modified apparatus is depicted in Fig. 1. In each experiment four quartz capillaries were filled with the molten alloy. A direct current was passed through two of the capillaries; the electrode in one of these capillaries was made the cathode, and the electrode in the other was made the anode. The remaining two capillaries sampled the alloy in the reser-

Jan 1, 1969

By A. C. Milner

In a gold standard world which possesses insufficient metal to meet the every-day needs of all, confidence becomes the vital factor, the very foundation upon which the machinery for the expansion of gold into currency, and credit, rests. The gold supply, affected by many influences, moves constantly from one point to another, but not always to that point where it is most needed. In the period 1928-1930, the combined gold holdings of the United States and France increased $1,370,936,-000, and this with new gold adding only $600,000,000 to the monetary gold stock.Theref ore, the gold stocks of other countries must have been depleted during the period by $770,936,000. This uncontrolled shifting throws the delicately adjusted instrumentalities of both credit and commerce out of equilibrium. If a given nation's gold stock shifts so as to bring it substantially below the legal reserve ratio set up against it for currency issues, the effect can easily extend to the currency issues and banking credit volume of one or more nations which may have based their gold exchange standards upon the gold stock of such nation. Thus the substitution of paper based on gold in place of the actual gold is an inflation of the currency, which carries through into an uncontrolled pyramiding upon the entire machinery of credit based on gold. In 1929 Europe, South America, Africa and Asia had overissued currency based on gold. America, Oceanica and Japan, which have not overissued their gold currencies, would in normal times require their entire present gold stocks and, as Continental Asia is largely upon a silver credit basis, from a domestic standpoint, it would appear that the gold problem is not so much one of maldistribution, as it is one of inadequate supply. It would appear that some method of increasing greatly the velocity of gold, within the safe reserve point, should be devised, or that silver, of which estimates indicate that 7,000,000,000 oz. are available for

Jan 1, 1931

By L. W. Holm

Laboratory flooding experiments on linear flow systerns indicated that high oil displacement, approaching that obtained from completely miscible solvents, can be attained by injecting a small slug of carbon dioxide into a reservoir and driving it with plain or carbonated water. Data are presented in this paper which show the results of laboratory work designed to evaluate this oil recovery process, particularly at reservoir temperatures above 100°F and in the pressure range of 600 to 2,600 psi. Under these conditions CO2 exists as a dense single-phase fluid. It was found that a bank, rich in light hydrocarbons, was formed at the leading edge of the CO? slug during floods on long cores. Formation of this bank is probably due to a selective extraction by the C02 and, it is believed, partially accounts for the attractively high oil recoveries. In crddition to the efficient displacernerlt of oil from the pores of the rock by this process, the favorable rnobility ratio related to a C0 2-water flood also contributes to high oil recovery. A further advantage of this process is noted on limestone and dolomite rock, in that the CO1 reacts with the porous medium increasing its permeability. Flooding experiments were conducted on sandstone and vugular dolomite models. The results of this experimental work show the effect on oil recovery of type of porous medium, pore geometry, flooding length, and flooding pressure. The porosity of the cores and rilodels varied from 16 to 21 per cent and their pern~eabilities ranged from 100 to 200 md. A reconstituted West Texas reservoir oil, a West Texas stock tank oil, an East Texas stock tank oil and Soltrol were used to represent reservoir oils in this study. Oil recoveries ranging from 60 to 80 per cent of the original oil in place in these cores were obtained by CO2,-carbonated water floods at pressures between 900 and 1,800 psi, compared with conventional solution gas drive and water-flood recoveries of 30 to 45 per cent on the same cores. Oil recoveries greater than 80 per cent resulted frorn f1oods at pressures above about 1.800 psi. There high recoveries were noted from both the sandstone and the irregular Porosity carbonate cores. In all floods, additional oil was recovered by a solutiorr gas drive resulting from blowdown following the flood. Oil recoveries of 6 to 15 per cent of the original oil in place were obtained during this blowdown period. This additional recovery was found to be a function of oil remaining after the flood, decreasing with decreasing oil saturation. It was also noted that highest oil recoveries by blowdown were obtained when carborlated water rather than plain water followed the CO, slug. INTRODUCTION Miscible phase or solvent flooding processes, which are designed to increase oil recovery -from petroleum reservoirs, involve the injection of small quantities of a petroleum solvent into the reservoir, followed by an inexpensive scavenging fluid which is miscible with the solvent. Essentially complete displacement of oil from the pores of reservoir rock has been obtained by this technique. CO,, although not completely miscible with most reservoir oils at moderate pressures, is highly soluble in these oils at pressures above about 700 psi; there is appreciable swelling and reduction in the viscosity of oil when CO, is dissolved in it. Therefore, CO, could be expected to perform similarly to other oil solvents as a displacing agent. CO, is also highly soluble in water at elevated pressures, so water should be a satisfactory material to drive a slug of CO, through an oil-bearing reservoir. A favorable mobility ratio would be obtained through the reduction in viscosity of the oil and the use of water as a final displacing agent. A number of investigations of the use of CO, to improve oil recovery have been reported in the literature.2,3,4,5,6 These studies, however, have been conducted on uniform porosity sandstone at relatively low temperatures and pressures. The behavior of CO1 as a flooding agent at temperatures above its critical temperature could not be predicted adequately from these studies, particularly for the case of non-homogeneous rock. The purpose of this work was to evaluate the oil recovery efficiency of a process involving the injection of a CO2 slug followed by carbonated water, at reservoir temperatures above 100°F and in the pressure range of 600 to 2,600 psi, and to compare this process with conventional water flooding. The investigations were primarily designed to provide information on the efficiency of the process in irregular porosity carbonate rock. The effects of flooding path length, the presence of free gas, the type of oil to be recovered, and the amount of solvent required were also determined. The essential results of static phase behavior studies and experimen-

H. W. MussEn, Collingwood, Ontario, Can. (communication to the Secretary*):—Doubtless all engineers who have paid more than a casual visit to Russia have come into contact with that formidable document, the " smieta," or estimate of the Russian manager. It is an institution which seems to be inseparable from Russian mining-methods. As Mr. Shockley points out, the year's costs a agree very closely" with the figures of the smieta made at the beginning of the year. In cases which have come under my notice, I have been satisfied that there had been a good deal of " rigging" of accounts to this end. The sum spent by the manager was carefully kept down to the total of the estimate, because it was well known that no more money would be forthcoming, and when this is done it is not a difficult matter to see that the right amounts come under the right heads in the final accounts. I do not say that this is always the case, but I have come across notable instances. Looking at it from the Russian owner's point of view, I think that the balance of the argument is usually in favor of the smieta as limiting " impulsive indiscretion" on the part of managers. The Russian Mining Code of to-day leaves much to be desired, but this is thoroughly appreciated by the official world there, and great changes are spoken of for the future. In many, if not in most, cases the laws are interpreted liberally, and a great deal is left to the discretion of the district mining engineer or inspector, with whom it is necessary to keep in close touch. As Mr. Shockley points out, the officials of a mine, who are always Russians, are held personally responsible for accidents resulting to employees, quite independently of any compensation which may be made to the sufferer. This seems startling enough, but I have always found that a penalty is imposed only

Jan 1, 1909

Jan 1, 1985

By R. O. Williams

It is shown that Ni3Al precipitates homogeneously from nickel-rich alwminum alloys as plates on the (100) planes. Prior to actual precipitation a process occurs which is believed to be one of increasing short-range order. After precipitating the Ni3Al plates enlarge through competitive growth. Discontinuous precipitation can occur simultaneously with the above processes. Recent ideas of the origin of precipitation strengthening appear adequate to explain the hardness changes. REMARKABLY little appears to be known about the precipitation process in Ni-Al alloys in spite of their technical importance. This investigation originated to supply additional information about precipitation in general, this system in particular. Information on the structures and kinetics have been obtained through the use of hardness, X-rays, microscopy, calorimetry, and resistivity on high-purity alloys. PROCEDURES Six alloys, Table I, were prepared by melting carbonyl nickel and high-purity aluminum in alumina crucibles in vacuum and casting into 1-in. graphite molds. All rods were homogenized at least once at 1300°C for 24 hr prior to swaging and this was repeated on the first three alloys after 75 pct reduction. Alloy 4 could be reduced only 10 pct at 1000°C (probably in two-phase field) prior to fracture but 1/4-in. samples quenched from 1100°C were readily reduced cold. Alloy 5 was reduced 15 pct cold but failed on the next pass while alloy 6 of essentially the same aluminum content failed inter-granularly without apparent flow up to 1000°C. The alloys were heated in hydrogen at the elevated temperatures and formed thin, coherent aluminum oxide coatings which provided excellent oxidation resistance at lower temperatures. However, freshly prepared surfaces showed considerably less resistance at 500"to 700°C in air and apparently resulted in internal oxidation. As a consequence, low-temperature agings were carried out in evacuated tubes. RESULTS The isothermal hardening behavior of these alloys at 500"and 565C is given in Figs. 1 and 2. These results were obtained from samples cold worked 75 pct, recrystallized at 1000°C (1100°C for the 7.8 pct Al) and quenched in water. This recrystallization was used to give smaller grain sizes so as to obtain more uniform hardness values and the points represent an average of five readings. The electrical resistivity was measured on 1/16-in. wires quenched from 1000°C during aging at 495°C to give Fig. 3. The energy release and its rate are given in Fig. 4 for the 6.9 pct Al alloy during aging around 500°C. Inasmuch as this was a single run, its accuracy is not known but certainly the general shape and magnitudes are correct. The method used to obtain these results is described elsewhere.' Data for the aging at 600°, 700°, and 800°C of these alloys cold worked 50 pct are given in Fig. 5. Supplementary information from microscopy and X-ray diffraction have been included to indicate recrystallization, discontinuous precipitation and the appearance of superlattice lines from the Ni3Al. The hardness of these alloys as annealed, aged, cold worked, and cold worked and aged is given vs composition in Fig. 6. Those samples which were isothermally aged, Figs. 1 and 2, were reaged at 532°C and at successively higher temperatures for the indicated times to give the data of Fig. 7. These results as well as certain others, support the idea that the level of hardness reached for temperatures above 600°C are equilibrium values more or less independent of path. This being the case, the breaks in the curves would be the complete solution of the Ni,Al. The electrical resistivity versus temperatures for some of these alloys, both aged and unaged, is given in Fig. 8 along with those data from heating slowly (10 deg per day) to high temperatures. Interesting points include the lowering of the Curie temperature (the change in slope), the lack of any indications of a solubility limit and the large temperature coefficient for the Ni3Al. A slight break for Ni3Al around 100C shows up but this is not a Curie temperature as Ni3Al is not ferromagnetic down to -190°C. Metallographically both the nickel-rich solid solution and the Ni3Al appear very much like pure nickel. Profuse twin boundaries are present both

Jan 1, 1960

By Marcel Schlumberger

The electrical methods for surface-prospecting have been well developed in the last 20 years. The method involves, in the classic form, the sending of an electrical current into the soil, by means of two electrodes A and B, and studying the potential distribution at the surface, by measuring the difference of potential between pairs of points such as M and N. The points M and N are usually placed on a line between, and equidistant from, A and B. By increasing the distance AB, the current sent into the Earth, and likewise the distribution of surface-potentials, become influenced by regions of greater and greater depth below the surface. By varying the form and dimensions of the electrode-arrangements AMNB, called a "quadripole," one may make valuable deductions concerning the nature or thickness of beds, if one knows the electrical properties of these beds. On the other hand, if the form and dimensions of the electrodes AMNB remain fixed, the depth of penetration of currents in the Earth remains, so to speak, almost constant, although it tends to increase where the subsoil is more conductive, and conversely. Therefore, if one moves the constant-dimension quadripole over all the terrain to be Investigated, one achieves approximately a horizontal exploration. This permits a study of tilted beds or faulted horizon-tal beds. When the particular problem becomes deep, of the order of 2000 meters, or more, it is ne-cessary to Increase the distance between the current-sources AB to a length such that the work 'comes very troublesome, especially if the region is wooded. At the same time, the separation the points M and N must be likewise great (for example, one km) in order to obtain differences potential which are not too small; the measurement of potential differences across MN is then difficult because of the presence of parasitic potentials, due to a flow of telluric currents in fourth, and the order of greatness of these currents may exceed the quantities to be measured.

Jan 1, 1940

By L. R. Jackson, W. T. Lankford, K. F. Smith

ComMercial steel sheet is prepared by a combination of hot and cold rolling and annealing. This treatment usually results in more or less pronounced anisotropy. The anisotropy may manifest itself both as preferred orientation and in the manner in which impurities, segregations, and the like, are aligned in the sheet. The type of preferred orientation and the organization of impurities or segregations may affect the elastic moduli, the yield strength, the tensile strength, and almost always the amount of ductility in different directions. In any case, the most important directions concerned in the anisotropy are along the rolling direction, along the width direction, and along the thickness direction. Considerable data exist on the anisot-ropy of sheet steel as demonstrated by conventional tensile tests; however, few attempts have been made to measure the constants of plastic anisotropy and use them to describe the flow of anisotropic sheet under combined stresses. In this paper, evidence is presented indicating that plastic flow in anisotropic sheet can be described by the shear-strain energy flow theory provided that the anisotropy is properly taken into account. Materials Used in the Investigation Table I lists the sheet materials used in this investigation and describes the condition in which materials were tested. Direction, of Tests and Test Methods Two types of tests were run—tensile tests and hydraulic-bulge tests. Characteristic parameters of anisotropy were determined from the tension tests by methods which will be described later. In all cases, the tensile test pieces were cut from the same quarter line and adjacent to the bulge test pieces in the sheet in order to minimize

Jan 1, 1949

By G. R. Speich, D. J. Mack

The transformation of was studied by isothermal methods. At all temperatures, the ß transforms quickly to fine grained ß" which develops silver-rich striations. At higher temperatures the striations disappear, the final structure being Widmanstatten a in ß'. At lower temperatures, the striated ß" is consumed by pearlite nodules of a + ß' which in turn form the Widmanstatten a in ß'. The transformation is unlike any previously reported for a eutectoid. AS part of a general program of study on the eutectoid reaction, the Ag-Cd eutectoid seemed particularly attractive because the ß phase which undergoes the reaction is another of the typical "electron compounds," AgCd, having the disordered body-centered cubic structure. This work deals with the eutectoid which occurs at 50.5 wt pct Ag, and not with the eutectoid which has been reported at 42.9 pct Ag.' There has been no work reported specifically on the Ag-Cd eutectoid which was studied. The only information available on this eutectoid is that work done in the determination of the phase diagram. For the most part, the terminal portions of the diagram, Fig. 1, are well established; however, the region from 40 to 60 pct Cd is still somewhat in doubt. The X-ray evidence'..' in this region is in conflict with the results of thermal analysis. X-ray analysis3 does not show a polymorphic transformation at about 240°C as indicated by thermal analysis.1,5 Even the X-ray evidence, within itself, is confusing in this region of the diagram. One investigator2 reports the ß phase as hexagonal close-packed and has found three phases in the one-phase ß field. Other X-ray investigators"' ' report the ß phase as body-centered cubic. The authors believe that much of the confusion resulted from incomplete homogenization of the alloys. It was found that it takes almost a week to produce a completely homogeneous two-phase structure at 370°C. Another possible source of error is the volatilization of cadmium from the surface and cracks of the specimen during annealing with the possible formation of a cadmium-poor phase. The only metallographic data available on this eutectoid alloy are those of Durrant1 and Fraenkel and Wolff.5 his information is very limited. The phase diagram chosen as most nearly correct is that in the Metals Handbook," which is almost identical with the phase diagram suggested by Durrant.1 Materials and Procedure The alloy was prepared from high purity silver (999.5 plus fine) and high purity cadmium (0.02 Pb, 0.005 Cu, trace Fe). The metals were melted in carbon under a nitrogen atmosphere. Some cadmium was lost by volatilization but by remelting several times and adding cadmium a 200 g ingot of approximately eutectoid composition was obtained. Because the CdO fumes are quite toxic, the exit gas from the furnace was led through a water trap to condense the CdO. The ingot was homogenized at 650°C for 24 hr, no attempt was made to prevent decadmiumization. This resulted in a narrow decadmiumized rim on the ingot which was removed. Filings for analysis were obtained from cross sections of the ingot. Silver was determined by the Volhard thiocyanate method,? cadmium by difference. The ingot analyzed 50.8 pct Ag at the top of the ingot and 50.7 pct at the middle and at the bottom of the ingot. This alloy was only slightly hypo-eutectoid compared to the accepted value of 50.5 pct Ag and was used for the isothermal studies. It was felt that further attempts to adjust the composition might be futile because of the volatility of the cadmium. The ingot was sectioned to specimens approximately 3/4 x 3/4 x 1/8 in. These specimens were "austeni-tized" for 3 hr in air at 650°C to yield homogeneous ß and then quenched into a salt bath held at constant subeutectoid temperatures where the transformation

Jan 1, 1954

By W. L. Austin

The only essential difference among the three methods of collecting the precious metals from their low-grade ores by fusion is comprised in the nature of the vehicle in which those metals are concentrated. If lead- or coppper-ores are used, the processes are respectively lead- or copper-smelting; but when the sulphide of iron forms the matrix in which the gold and silver are collected, the process is known as pyritic smelting. The latter method presents rarely any advantages when lead- or copper-ores are available at rates which permit profitable treatment. Pyritic silver-smelting, defined by Percy as " the smelting of silver-ores, which are either free from lead or do not contain it in sufficient quantity to collect the silver, in conjunction with pyrites, in order to produce a regulus in which the silver may be concentrated," is not, as the name would imply, confined to ores of this metal alone, but embraces auriferous silver-ores, or even gold-ores simple. This method of collecting the precious metals from lowgrade dry ores, employed at Freiberg by Barthel Kohler in 1585, does not appear, up to the present, to have been introduced into this country on a working scale. And yet the possibility of getting rid in a single operation of all the earthy or siliceous gangue of a lowgrade ore and concentrating the precious metals in a matte without loss of lead (which includes gold and silver) by slagging, or volatilization, at the same time producing a highly siliceous slag, very nearly if not quite as clean as is usual in lead-smelting, certainly commends itself. In some parts of the country, owing to the com-

Jan 1, 1888

By C. W. Covington, H. C. Cook, J. F. Libsch

Sputtered aluminum thin films were prepared in each of two conventional bell-jar vacuum systems. One system utilized an inner "getter sputtering" enclosure; the second system was a standard diode sputterirlg arrangement. Consistent and repeatable film properties were obtained in both systems provided sufficient cleanup and presputter time was allowed. The various problems associated with aluminum sputtering are discussed, with pavticular attention to the vzinimization of film contamination by outgassing and oxidation. The growth and structure of the aluminum thin films were studied with the aid of electron wzicroscopy and related to deposition rate, substrate temperature, and film thickness. The resistivity of the films was correlated to film structure and surface roughness. Resistiuities as low as 3.5 microhm-cm (2.3 x bulk resistiuity) were measured for relatively thick films (20,000). THIS investigation was undertaken to explore the problems and film characteristics associated with the sputtering of aluminum. Earlier work reported on aluminum sputtering has stressed the contamination of both the cathode and film as well as abnormally low deposition rates.' Data on sputtering yields,3 however, indicate that aluminum sputtering could be practical. Recently, it was shown by Theuerer and Hauser3 that aluminum sputtering was feasible in a conventional oil-diffusion pumped vacuum system provided an inner "getter sputtering" enclosure was employed to minimize gaseous contamination. This technique employs the getter action of aluminum to produce extremely low reactive gas partial pressures in the deposition zone. Aluminum films have already found use in solid-state electronic devices such as transistors and integrated microcircuits. To the present time, most aluminum films have been prepared by evaporation due to the ease with which this metal can be evaporated. Controlled sputtering of aluminum offers a number of advantages over evaporation, however, such as 1) manufacturing compatibility with other metals which must be sputtered, 2) better control of process variables resulting in more repeatable and uniform films, 3) generally better adhesion resulting from higher-energy metal atoms, 4) built-in material supply for continuous operation, and 5) the ability to deposit alloys. The data presented in this paper are the result of two separate studies. One study utilized a small "getter sputtering" enclosure (System A) and was concerned with the structure and properties of thin aluminum films up to about 1600A thick. In this thickness range, study of the film structure was possible with transmission electron microscopy. The second study was conducted with a conventional diode sputtering apparatus (System B) and covered $ much wider range of film thickness up to about 34,000A. Emphasis was placed on developing techniques which would extend aluminum sputtering to an existing in-line continuous deposition process.4 I) EQUIPMENT AND PROCEDURE System A. Fig. 1 shows a schematic of the "getter sputtering" inner chamber used and Fig. 2 is a photograph of this chamber mounted on an 18-in. access ring of a standard liquid-nitrogen trapped bell-jar vacuum system. This chamber was designed after a similar system used by Theuerer and auser.3 The configuration allowed the glow to emanate in all directions from the cathode. Argon (99.99') was allowed to enter only at the top of the chamber such that most of the reactive gases entering with the argon were reacted with the aluminum vapor and deposited on the chilled walls of the chamber before reaching the deposition zone. Provision was also made as shown, Fig. 1, for heating and cooling the substrate from about 20" to 400°C. Two substrate materials were used: Corning 7059 glass (12 by 12 by 0.048 in.) and carbon films about

Jan 1, 1967

By J. E. Neal, C. T. Naber, O&apos

Silicon thin films were deposited by electron beam evaporation in an ultrahigh vacuum onto (0001) and (1102) sapphire substrates. Attempts were made to correlate the structural properties of the deposited silicon films with the following: 1) substrate orientation, 2) substrate surface condition, 3) substrate temperature, and 4) deposition rate. The substrate temperatures were varied between 500° and 1000°C and the deposition rates were varied between approximately 50 and 700A per min. The following sapphire surface treatments were investigated: 1) annealing in the ultrahigh vacuum at 1200° C; 2) heating in a hydrogen atmosphere at about 1350°C; and 3) etching with silicon by evaporating silicon onto sapphire substrates heated to 1200° or 1300°C. Twinned silicon films were occasionally formed at substrate temperatures between the 800° and 1000°C on unprocessed mechanically polished substrates; however, the reproducibility and crystallinity of these films were generally poor. Single-crystal and twinned silicon films were formed at substrate temperatures between 700° and 1000°C on substrates which were silicon-etched at 1300°C prior to deposition. Fiber texture films were formed at substrate temperatures between 500° and 700°C. The (111) lattice plane of the silicon single-crystal films was parallel to the (0001) sapphire plane and the (100) silicon plane was parallel to the (1102) sapphire plane. TECHNIQUES are well-established for growing single-crystal silicon thin films on sapphire by chemical methods.'-* Vacuum epitaxial techniques have a number of advantages over chemical epitaxial techniques in the fabrication of thin film microcircuits.5 One of the most significant is that vacuum techniques are compatible with well-established procedures for forming vacuum-deposited thin-film resistors, capacitors, and interconnections. Salatna, Tucker, and young6 recently reported the formation of relatively poor crystalline-quality silicon films on sapphire by electron beam evaporation in a vacuum of about 7 x 10-7 Torr. The purpose of the investigation described here is to determine the relationships between the structural properties of silicon thin films deposited on sapphire substrates by electron beam evaporation in an ultra-high vacuum and the following: 1) substrate orientation; 2) substrate surface condition; 3) substrate temperature; and 4) deposition rate. The substrate temperatures were varied between 500° and 1000° C and the deposition rates were varied between approximately 50 and 700A per min. Two orientations of sapphire were used: (0001) and (1102). The thick-nesses of the films were between 8000 and 16,000A. The morphology and crystallinity of the deposited films and substrate surfaces were investigated by optical microscopy, electron microscopy, and electron diffraction. APPARATUS AND PROCEDURE A cross section of the ultrahigh-vacuum thin-film evaporator is shown in Fig. 1. The bell jar is stainless steel and copper gaskets are utilized at all seals. High vacuum is attained by a 6001iter per sec ion pump and a titanium sublimation pump. Sorption pumps are used to rough the system to a pressure of about 10 µ prior to starting the ion pump. Vacuums in the 10- 10 Torr range were attained after baking the system at about 250°C for 8 hr. Vacuums in the 10-8 to 10-9 Torr range were maintained during silicon evaporation. The silicon charges, which were cut from p-type single-crystal boules which had resistivities between 2000 and 4500 ohm-cm, were placed in the water-cooled copper crucible of a 180 deg bent-beam 5-kw electron beam evaporator. During evaporation, a molten zone was formed in the top center of the silicon charge, and the portion of the silicon charge in contact with the water-cooled crucible remained solid. The substrate heater, which has been described

Jan 1, 1969

By Karl J. Dreher, Charles C. Hennig, Gregg A. Scott

INTRODUCTION Theodore Roosevelt Dam is a cyclopean-masonry, gravity-arch dam located on the Salt River northeast of Phoenix, Arizona. Construction of the dam began in 1903 and was completed in 1911. The dam is about 85 m high with a total reservoir capacity of about 1.7x109 m3. Raising the dam is now being considered to provide additional water storage and flood control. This paper describes preliminary analyses performed to assess foundation stability for increased loading resulting from raising the dam and reservoir water surface about 12 m. The foundation of Theodore Roosevelt Dam consists of variably metamorphosed limes tones, sands tones, mudstones, and shales. Bedding uniformly strikes nearly normal to the river (N 40º W) and dips upstream at 25 to 30º. The rock is cut by four prominent joint sets as indicated by the joint contour diagram shown in figure 1A. The diagram was developed from surf ace observations and vertical drill core oriented relative to the bedding. Sampling biases account for the differences in concentrations of various joint sets. However, field observations indicate that all sets are relatively prominent, planar, and continuous. SEEPAGE ANALYSES Consistent with practice at the time of construction, no foundation drainage was installed at Theodore Roosevelt Dam. Finite element seepage analyses were therefore performed to study the potential for large uplift pressures in the foundation. The dam has steep abutments and is curved in plan as shown in figure 1B. The effects of modeling the seepage two-dimensionally, radially symmetric about the dam's axis center, and three-dimensionally were therefore com-

Jan 1, 1982

By C. E. Corson

Discussion of the Paper by C. E. Corson, which was presented at the London Meeting, July, 1906. (See Bi-Monthly Bulletin, No. 11, September, pp. 725 to 742.) ALBERT SAUVEUR, Cambridge, Mass. (communication to the Secretary*) :-On close examination I think it will be found that the evidence by which Mr. Corson claims to have shown the inaccuracy of a statement I made a few years ago, is far from convincing. This statement is:- "Hot work, as such, has no influence upon the structure of the metal. Indirectly, however, by retarding crystallization until a lower temperature is reached, it may influence its structure most decidedly ; but the same results could be accomplished by heat-treatment alone, i.e., by reheating the unworked metal to the temperature from which the unworked piece was allowed to cool undisturbedly." The Metallographist, vol. ii., p. 267 (under the head of "Changes of Structure Brought About by Work"). Of the two pieces of steel tested by Mr. Corson, one was worked and finished at a " cherry red " and ' the other reheated to a cherry red, and the assumption was made that, in both cases the temperature was about 715° C., although no pyrometric device was used to record it. The possibility of considerable difference in temperature alone is so great as to invalidate Mr. Corson's inferences. The apparent temperature, moreover, is so close to the critical point of the steel as to render any conclusion very hazardous. -It is not at all evident that the annealed piece was reheated past its critical point, in which case reheating would have had practically no effect. Nor is it evident that the piece forged and finished at a cherry red was not actually below the critical point, which, by definition, I have called cold worked. Mr. Corson's explanation that " Under proper reheating, on the other hand, the steel becomes a solid solution from which crystals of approximate homogeneity and uniform size may separate" will not be readily understood.

Jan 1, 1907

By Jean Bonnemaison

Societe Miniere & Metallurgique de Penarroya Noyelles-Godault works are located in the northern part of France. The complex includes a lead smelter, a zinc smelter, shops for production of manufactured products and all necessary general services. The zinc smelting complex described in this paper was designed in 1959 to replace an old horizontal retort distillation furnace and was first operated in May 1962. It includes: - a sinter plant producing the zinc sinter for the Imperial Smelting furnace : zinc, lead and bulk zinc-lead concentrates are sintered on a Dwight-Lloyd machine with a working area of 80 sq.m. Cadmium sludges are treated by the wet method in a separate plant for recovery of cadmium. Sulphur dioxide contained in gases goes to a gas washing tower and is subsequently made into sulphuric acid in a plant with a capacity of 550 m.t. per day. - a smelting plant where the process developed by Imperial Smelting Processes Ltd. is applied : the blast furnace which was modified in 1967 has an area of 17.5 sq.m. at the tuyeres level and a section of 24 sq.m. at the top of the shaft. It has a theoretical zinc capacity of 100,000 m.t. per annum. Air blast is heated by means of covers up to the theoretical temperature of 950ºC. Zinc produced is either directly cast into slabs for sale as standard 'good ordinary brand' zinc, or sent to a refining plant where the New Jersey process designed to produce 'special high grade' zinc is in application. Mixes of zinc containing various amounts of lead, cadmium or aluminum are prepared to customer specification in a mixing plant.

Jan 1, 1970

By A. L. O’Neil, J. A. Wineland, A. B. Arnold

Movement of water through the Tehachapi Mountains was one of the most challenging parts of the planning, design, and construction of the California Aqueduct. The California Aqueduct is the main artery of the California State Water Project, which will move water 444 miles from the Sacramento-San Joaquin Delta into the arid and semiarid, densely populated parts of Southern California. The $2,000,000,000 project, designed and constructed by the California State Dept. of Water Resources, was started in 1957 at the Oroville Dam site and is now well past the halfway mark in construction. Water is now being delivered from the California Aqueduct to portions of the San Joaquin Valley. The California Aqueduct is scheduled for completion in 1972. Tunnels on the Tehachapi Crossing are often overshadowed in engineering descriptions of the Crossing by the tremendous importance and engineering significance of the Tehachapi pumping plant which will pump water through the tunnel system. For purposes of this paper, it will suffice to say that the plant is designed to lift 4100 cu ft of water per sec up approximately 2000 ft, making this the highest pumplift in the United States and one of the largest in the world. Water will be moved from the pumping plant through twin tunnels called the Tehachapi Discharge Lines to the top of the lift. From here, water will flow through four additional tunnels which are all linked by short connecting structures (Fig. 1). The tunnels are referred to as Tunnels 1, 2, 3, and Carley V. Porter Tunnel. HISTORY Selection of the final route of the Tehachapi Crossing was the result of comprehensive investigations beginning in 195 1. Numerous tunnel

Jan 1, 1970