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By A. U. Seybolt, Bruce W. Gonser

A few copper-zinc-hasp alloys mppt die-casting requirements reasonably well, although improvements are desired. Aluminum bronzes, high-tin bronzes and some copper-nickel-zinc alloys can be die-cast, according to Herb,' but seldom are because of such factors as higher melting ranges and greater cost than certain of the brasses. Fox2 has summarized the copper-base die-casting alloys that were in commercial use in 1937 and has given the effects of different alloying constituents. Table 1 gives some of the properties of these alloys as reported by Fox. a Properties reported by Fox.2 b Trade name of Brastil, Doehler Die Casting Co., similar to Webert Alloy,34 American Brass Co., and Tombasil Alloy,5 Ajax Metal Co. e Trade name Tinicosil, Titan Metal Manufacturing Co. Melting point (liquidus) of the yellow brass is given by Herb1 as 1650" F., of the high-silicon Brastil (with 4.5 to 5 per cent Si) as 1600" F., and of the nickel silver as 1675" F. d Criterion not stated.

Jan 1, 1940

By Cyril Stanley Smith

On the 6th of February 1684, Dr. Martin Lister mentioned at a meeting of the Royal Society1 that "brass is magnetical," and promised to give an account of that assertion at some other time. He repeated his promise but never fulfilled it, and it was left for William Arderon2 to show, in 1758, that brass could be made magnetic by hammering and that it would retain polarity after magnetizing. Twenty-seven years later Caval103,4 examined the matter in great detail. Working with cast calamine brass, he showed that it could be made magnetic by hammering and nonmagnetic by subsequent annealing at a red heat. He found that annealing at a very high temperature caused the samples to lose their magnetic quality permanently, even after subsequent cold-working, but that remelting and cold- working restored it. He encountered some samples of brass that could not be rendered - magnetic by any treatment. Experiments in which these were remelted with iron additions gave negative results, and Cavallo concluded that iron impurity was not the cause of the magnetism. He worked with 50-grain (3-gram) samples melted under the blowpipe, hence cooled very quickly. Bennet5 made whole crucible charges from copper and zinc, and found _ the resulting brass ingots to be magnetic only when iron had been added and then only after cold-working. All these observations applied to material in the cast condi- tion, in which coring would produce a continuous spectrum of composition and cooling would result in varying degrees of precipitation. This knowledge of the subject seems to have been forgotten in the nineteenth century. The older brass was made by the calamine process and frequently contained iron in amounts of 0.5 per cent or more, absorbed from the impure ore with which the copper and charcoal were heated in making the brass. When metallic zinc became available in commercial quantities, calamine brass gradually disappeared, and with it the knowledge of its curious magnetic properties. Only when sensitive apparatus replaced the compass needle of the earlier investigators could the effects be detected in relatively pure metal. The effect of cold-working in inducing ferromagnetism was rediscovered by Bitter8 in 1930 in a sample of impure copper, and this was confirmed by Lowance and Constant: Honda and Shimizu, l0,11 and others. In the same year, Tammann and Oelsen12 showed that copper-rich copper-iron alloys after certain heat-treatments could be rendered ferromagnetic or made more strongly ferromagnetic by cold-rolling. Kussman and Seeman13 showed that the change of susceptibility of relatively pure copper on cold-working was associated with the iron content, and concluded that actual precipitation of iron was caused by cold-working, which is a satisfactory theory until one considers the improbably high rate of diffusion that this would involve. When studying precipitation phenomena in

Jan 1, 1942

By Cyril Stanley Smith

On the 6th of February 1684, Dr. Martin Lister mentioned at a meeting of the Royal Society1 that "brass is magnetical," and promised to give an account of that assertion at some other time. He repeated his promise but never fulfilled it, and it was left for William Arderon2 to show, in 1758, that brass could be made magnetic by hammering and that it would retain polarity after magnetizing. Twenty-seven years later Caval103,4 examined the matter in great detail. Working with cast calamine brass, he showed that it could be made magnetic by hammering and nonmagnetic by subsequent annealing at a red heat. He found that annealing at a very high temperature caused the samples to lose their magnetic quality permanently, even after subsequent cold-working, but that remelting and cold- working restored it. He encountered some samples of brass that could not be rendered - magnetic by any treatment. Experiments in which these were remelted with iron additions gave negative results, and Cavallo concluded that iron impurity was not the cause of the magnetism. He worked with 50-grain (3-gram) samples melted under the blowpipe, hence cooled very quickly. Bennet5 made whole crucible charges from copper and zinc, and found _ the resulting brass ingots to be magnetic only when iron had been added and then only after cold-working. All these observations applied to material in the cast condi- tion, in which coring would produce a continuous spectrum of composition and cooling would result in varying degrees of precipitation. This knowledge of the subject seems to have been forgotten in the nineteenth century. The older brass was made by the calamine process and frequently contained iron in amounts of 0.5 per cent or more, absorbed from the impure ore with which the copper and charcoal were heated in making the brass. When metallic zinc became available in commercial quantities, calamine brass gradually disappeared, and with it the knowledge of its curious magnetic properties. Only when sensitive apparatus replaced the compass needle of the earlier investigators could the effects be detected in relatively pure metal. The effect of cold-working in inducing ferromagnetism was rediscovered by Bitter8 in 1930 in a sample of impure copper, and this was confirmed by Lowance and Constant: Honda and Shimizu, l0,11 and others. In the same year, Tammann and Oelsen12 showed that copper-rich copper-iron alloys after certain heat-treatments could be rendered ferromagnetic or made more strongly ferromagnetic by cold-rolling. Kussman and Seeman13 showed that the change of susceptibility of relatively pure copper on cold-working was associated with the iron content, and concluded that actual precipitation of iron was caused by cold-working, which is a satisfactory theory until one considers the improbably high rate of diffusion that this would involve. When studying precipitation phenomena in

Jan 1, 1942

By R. W. Gurry

IN the course of a series of measurements of the rate of diffusion of carbon in austenite at about 960°C. (1760°F.) and 1110°C. (2030°F.), it became necessary to determine carbon concentration when austenite is saturated with graphite, because of indications that the hitherto accepted value of the solubility of graphite in this temperature range is too low. Specimens of carbonyl iron were saturated at temperature in a hydrogen-toluene atmosphere which was in equilibrium with graphite. The carbon content of the steel was measured either by combustion or by the loss of weight after substantially complete decarburization in an atmosphere of hydrogen saturated at room temperature with water vapor. The absence of carbide or graphite as a phase at temperature was demonstrated by microscopic examination of saturated specimens that had been drastically quenched. The mean result of concordant measurements is that gamma iron saturated with respect to graphite contains 1.39 per cent carbon at 957°C. (1755°F.) and 1.89 per cent at 1110°C. (2030°°F.). These two values, plotted along with what appears from the literature to be the best value (0.69 per cent) at the iron-graphite eutectoid temperature (738°C. or 1360°F.), yield a curve that is almost linear, and which, continued upward through a short interval, leads to a limiting solubility of 1.98 per cent at the iron-graphite eutectic temperature1135°C. (2095°F.) instead of the commonly accepted value of about 1.7 per cent. EXPERIMENTAL PROCEDURE The samples of carbonyl iron, with the exception of those for microscopic examination, were cylinders 3.8 cm. long, 0.475 cm. in diameter. They were placed in a graphite holder and suspended in a vertical furnace, the temperature of which was controlled precisely by means of the resistance of the platinum winding.1 In the empty furnace the range of temperature over a distance of 4 cm, at the heat center was 9°C. (16°F.) but at a given location the temperature remained within ±0.5°C. (0.9°F.); it was measured by inserting a platinum-rhodium couple calibrated at the melting point of palladium, 1555°C. Since the presence of the sample probably improved the uniformity of temperature, it was decided to consider the average temperature of the sample to be 3°C. lower than the maximum measured in the empty furnace with the same setting of the controller. Data were obtained in the vicinity of two temperatures, 960°C. (1760°F.) and 1110°C. (2030°F.). The samples for microscopic examination, 2.2 cm. long, 0.475 cm. in diameter, were suspended individually on pure iron wire; for these no temperature correction was applied. The carburizing gas passed into the furnace was dry, oxygen-free hydrogen saturated at room temperature with

Jan 1, 1942

By John W. Crutchfield, Emil F. Bowers

This paper presents the initial results of a pressure maintenance by water return project in the Lower Pawelek reservoir of the Falls City Field, Karnes County, Southwest Texas. Production is from the Lower Wilcox section at an average depth of 6,030 ft on the downthrown side of a "down to the coast" fault. Of particular interest is that the reservoir oil is high gravity and low viscosity but far undersaturated with gas at the original reservoir pressure and temperature. The early pressure and production history indicated only a partial or limited water drive, and this fact, coupled with the characteristics of the reservoir fluid and artificial lifting problem.. made advisable the water injection program to maintain reservoir pressure. The paper includes a description of the reservoir and reservoir fluids, the pressure and production history, a description of the water injection facilities, and the results of reservoir calculations involving Hurst's unsteady state flow and the material balance equations for calculation of water influx and prediction of the pressure-production relationship at various rates of withdrawal. The reservoir calculations and initial field results indicate that reservoir pressures in excess of 85 per cent of original pressure can be maintained by control of water injection even at very high rates of production. INTRODUCTION The purpose of this paper is to report the initial results of a pressure maintenance by water return program in the Lower Pawelek reservoir, Falls City Field, Karnes County. Texas, and to calculate an empirical relationship between pressure and production in this limited or partial water drive reservoir. Location The Falls City Field (Fig. 1) is located two miles north of the town of Falls City in Karnes County, Texas, and is approximately 50 miles south-southeast of San Antonio on U. S. Highway 181. Discovery and Development The initial block of leases was taken after a surface geological survey identified a major east-west fault and closure on the south or downthrown section. The discovery well, Southern Minerals Corporation's Joe F. Bartosch 1; was completed at 4,650 ft in the Lower Bartosch sand in December, 1944. Drilling was continuous until December, 1946, and resulted in the discovery of 12 oil reservoirs between 4,600 and 6,050 ft in the Middle and Lower Wilcox formations. These are shown on the cross-section (Fig. 2). As of the current date there are 64 oil wells completed as follows: Southern Gulfshore Magnolia Minerals Oil Petroleum Reservoir Corp. Co. Corp. Total Upper Bartosch 0 0 0 0 Lower Bartosch 16 0 0 16 Shulze 7 0 1 8 Upper Faires 2 0 0 2 Lower Faires 4 0 0 4 Upper Moczygemba 0 0 0 0 Lower Moczygemha 2 0 0 2 Olinick 2 0 0 2 Upper Martinez 0 0 0 0 Lower Martinez 5 0 0 5 Upper Pawelek 0 0 1 Lower Pawelek 27 1 3 31 Total 65 2 4 71

Jan 1, 1950

By J. R. Cahoon, W. V. Youdelis

FOR the diffusion of copper in silver-rich alloys, there have been only two previous investigations, that of Seith and Peretti in 1936, and that of Sawatzky and Jaumot2 in 1957. Seith and Peretti obtained a value of 24.8 keal per g-atom for the activation energy of diffusion whereas Sawatzky and Jaumot obtained a value of 46.1 keal per g-atom. Admittedly, Seith and Peretti used relatively high concentrations of 2 at. pet Cu and polycrystalline diffusion couples, while Sawatzky and Jaumot investigated tracer diffusion in single crystals of silver. The difference in the results, however, seems too large to attribute solely to solute concentration, as a change of over 20 keal per g-atom in the activation energy suggests a change in the mechanism of diffusion. Therefore, in the present investigation the diffusion coefficient for copper in polycrystalline Ag-2 at, pet Cu alloy is re-established using conventional sandwich-type diffusion couples and electron-probe microanalyses, and the results are compared with those of the previous studies. The diffusion couples were prepared from high-purity silver (99.999 pet) and high-purity copper (99.999 pet). The silver disks, 1/4 in. long and 4 in. in diam, were machined from an ingot which had been solidified in a dynamic vacuum of 10-3 mm of Hg to eliminate oxygen absorption which otherwise would result in copper oxide precipitation in the weld zone. The alloy disks of similar dimensions were machined from an alloy ingot (nominal composition 2 at. pet Cu) which had been unidirectionally solidified to obtain a predictable solute concentration,3 and homogenized for 1 week at 800°C. Sandwich diffusion couples were made by pressure welding an alloy disk between two silver disks in an induction heating coil. The couples were diffusion-annealed at temperatures of 800°, 756°, 699°, and 630°C in tube furnaces in which the temperature was controlled to better than ± l°C. The diffusion couples were examined metallographically for weld defects, and couples showing even minute defects at the weld interfaces were rejected. Concentration penetration curves were established using an A.R.L. Microprobe analyzer. CuKO radiation was counted and converted to concentration using 0.5 and 1.0 wt pet Cu chemically analyzed standards. Initially, four continuous profiles were obtained, and averaged to obtain the final diffusion curve. The initial analysis was performed commercially and the welds were not located with respect to the profile. Therefore, the results were rechecked by the authors using the Mellon Institute A.R.L. probe. In the latter case, concentrations were obtained at 10-µ steps for four different traverses, and then averaged to obtain

Jan 1, 1968

By D. P. Pope, T. Vreeland

Observations of dislocations in zinc using Berg-Barrett X-ray micrography confirm the validity of a dislocation etch for (1010) surfaces. A technique for measurement of the depth in which dislocations can be imaged in X-ray micrographs is given. This depth on (0001) surfaces of zinc was found to be 2.5 µ using a (1013) reflection and CoKa radiation. BUCHANAN and Reed-Hill (B & RH) have recently questioned the ability of a dislocation etch to reveal all of the basal dislocations which intersect (1010) surfaces in annealed zinc crystals.' This etch was developed by Brandt, Adams, and Vreeland who conducted a number of different experiments to check its ability to reveal dislocations.2,3 B & RH prepared (0001) foil specimens for transmission electron microscopy from annealed crystals and observed dislocation densities of about l08 cm per cu cm in the foils, while the etch indicated densities of the order of l04 cm per cu cm in their annealed crystals. As this etch has been used in a number of studies of dislocations in zinc, it is of considerable importance to reassess its validity in the light of the B & RH results. The X-ray work reported here was undertaken to check the ability of the etch to reveal dislocation intersections on (1070) surfaces of zinc. The X-ray technique was chosen for this check because it could be applied to the as-grown crystals with a relatively small amount of specimen preparation. We believe that the possibility of accidental deformation in preparation of the bulk specimens is considerably less than that for thin foil specimens suitable for transmission electron microscopy. Unfortunately, basal dislocations are not visible on Berg-Barrett topo-graphs of (1010) surfaces, which are the surfaces on which the etch is most effective. Therefore, a one-to-one correspondence between the etch and X-ray observations could not be made. Basal dislocations near (0001) surfaces have been observed by Schultz and Armstrong4 using the Berg-Barrett technique, but they did not report the as-grown dislocation density observed in their crystals. We have applied the X-ray technique in this study to surfaces oriented from 1 to 2 deg of the (0001) to determine the basal dislocation density, and have compared this density with that observed using the etch on a (1070) plane of the same crystal. The X-ray observations permit determination of the depth in which basal dislocations can be observed under the diffracting conditions used. SPECIMEN PREPARATION High purity zinc crystals are very soft, so a good deal of care must be exercised in the preparation of observation surfaces. As-grown crystals approximately 2.5 cm in diam and 20 cm long were acid cut into 1.25 cm cubes. A thin slab was cleaved from an (0001) surface to produce an accurately oriented reference surface on the specimen. Some of the cubes were examined in the as-machined condition while some were annealed in argon at 410°C for 2 hr. Heating and cooling rates were less than 2°C per min. Some of the specimens were scratched on a (0001) surface with a razor blade to produce fresh dislocations. Approximately 2 mm of material was acid lapped from one face of a cube to produce a surface oriented between 1 and 2 deg from the basal plane and parallel to the [1210] direction. A (1070) surface was also acid lapped. The lap used a 1 to 3 pct solution of HN03 in water to saturate a soft cloth which was backed by a stainless steel plate. The cloth was moved over the crystal surface at a rate of 20 cm per sec while a normal force of about 4 g was maintained between the cloth and the specimen. As-lapped surfaces were examined as were surfaces which were chemically and electrolytically polished after lapping. The small angle between a lapped surface and the (0001) plane was measured to 0.1 deg using a Unitron microgoniometer microscope (the cleaved surface was used as a reference in this measurement). The microscope was modified so that the intensity of reflected light could be continuously monitored on a meter. This modification produced nearly a ten-fold increase in the reproduceability of orientation readings. OBSERVATIONS The Unitron Microgoniometer observations indicated that the lapped surfaces had a terraced structure with the terraces quite rounded and spaced about 0.1 mm in the [1010] direction. The maximum change in slope between terraces was 0.25 deg, indicating a terrace height of about 0.1 µ. A Unitron measurement of the average angle between (0001) and a lapped surface was checked by micrometer measurement of the specimen and found to agree within 0.1 deg. The Berg-Barrett micrographs using (1013) reflections and CoKa radiation5 revealed subboundaries, short dislocation segments, spirals, and loops near the surfaces which were oriented from 1 to 2 deg of the (0001). Micrographs of surfaces prepared by lapping appeared very similar to those of the chemically and electrolytically polished surfaces. The loops and spirals were not extinct in (1013) or (0002) reflections, indicating that they have a nonbasal Burgers vector. Extinctions of the short, straight dislocations indicated that they belonged to an (0001)(1210) system. Fig. 1 is an example of a micrograph which shows a subboundary, and dislocation segments which are pre-

Jan 1, 1970

By Coleman D. Hunter, George M. Straughan

Oil and gas development as well as extensive leasing in Kentucky during 1940 has shown a marked improvement over the past three years.$ The most noticeable improvement is the gas development in eastern Kentucky and the deep tests being drilled by major oil interests. In western Kentucky, 406 wells were drilled, of which 173 were oil producers, 12 were gas wells and 221 were dry or abandoned. The number of dry tests was large, because no important, new oil or gas pool was discovered and many of the dry holes could be considered wildcat tests. However, with either oil or gas possibilities from Pennsylvanian formations on through Mississippian, Silurian, Devonian, and Ordovician, this percentage of dry holes seems rather high. Many of the dry tests possibly should have been tested in deeper horizons before being abandoned: namely, Silurian and Ordovician ages. In eastern Kentucky, 213 wells were drilled, of which 113 were gas producers, 61 were oil wells, and 39 were dry holes. Of these wells, 117 were drilled in the most important Big Sandy gas field, in Floyd, Pike, Knott and Martin Counties, and of this number 103 were gas producers, 5 were oil wells, and 9 were dry holes. In the Big Sinking oil field of Estill, Lee and Powell Counties, 70 of the remaining 96 wells were drilled, j6 being oil producers. During 1940, four deep tests were drilled in eastern Kentucky. One test penetrated the Knox dolomite in Knox County and was dry; no St. Peter sand was encountered. Another test in Lee County had some gas in what might be called St. Peter sand, according to the State Department, and also some gas deeper in the Knox dolomite. In Wolfe County, a small oil well was completed in the Ordovician, which was undoubtedly of Trenton age. ilt the present time, four deep tests are being drilled, all of which will go to the Knox dolomite. In Elliott County, on the Burke dome, the Inland Gas Co, is drilling at 3650 ft. In Magoffin County, on the Paint Creek uplift, the Cumberland Petroleum Co. is drilling at 3800 ft. In Clark County, in the Ruckerville fault area, W. 0. Allen is drilling at 1800 ft. In Laurel County, on the Sinking Creek dome, the Globe Oil and Gas Co. is drilling at I750 ft. If production is encountered in the Trenton, St. Peter, or Knox dolomite in any of these tests, eastern Kentucky will experience a marked increase in deep development.

Jan 1, 1941

By George M. Straughan, Coleman D. Hunter

Oil and gas development as well as extensive leasing in Kentucky during 1940 has shown a marked improvement over the past three years.$ The most noticeable improvement is the gas development in eastern Kentucky and the deep tests being drilled by major oil interests. In western Kentucky, 406 wells were drilled, of which 173 were oil producers, 12 were gas wells and 221 were dry or abandoned. The number of dry tests was large, because no important, new oil or gas pool was discovered and many of the dry holes could be considered wildcat tests. However, with either oil or gas possibilities from Pennsylvanian formations on through Mississippian, Silurian, Devonian, and Ordovician, this percentage of dry holes seems rather high. Many of the dry tests possibly should have been tested in deeper horizons before being abandoned: namely, Silurian and Ordovician ages. In eastern Kentucky, 213 wells were drilled, of which 113 were gas producers, 61 were oil wells, and 39 were dry holes. Of these wells, 117 were drilled in the most important Big Sandy gas field, in Floyd, Pike, Knott and Martin Counties, and of this number 103 were gas producers, 5 were oil wells, and 9 were dry holes. In the Big Sinking oil field of Estill, Lee and Powell Counties, 70 of the remaining 96 wells were drilled, j6 being oil producers. During 1940, four deep tests were drilled in eastern Kentucky. One test penetrated the Knox dolomite in Knox County and was dry; no St. Peter sand was encountered. Another test in Lee County had some gas in what might be called St. Peter sand, according to the State Department, and also some gas deeper in the Knox dolomite. In Wolfe County, a small oil well was completed in the Ordovician, which was undoubtedly of Trenton age. ilt the present time, four deep tests are being drilled, all of which will go to the Knox dolomite. In Elliott County, on the Burke dome, the Inland Gas Co, is drilling at 3650 ft. In Magoffin County, on the Paint Creek uplift, the Cumberland Petroleum Co. is drilling at 3800 ft. In Clark County, in the Ruckerville fault area, W. 0. Allen is drilling at 1800 ft. In Laurel County, on the Sinking Creek dome, the Globe Oil and Gas Co. is drilling at I750 ft. If production is encountered in the Trenton, St. Peter, or Knox dolomite in any of these tests, eastern Kentucky will experience a marked increase in deep development.

Jan 1, 1941

SECTION I Page Page Manuscript Closing Date, Febru- Forthcoming Meetings xxvii ary Meeting v . Library xxviii New York Section War Meeting on Membership xxxii Ferro-Alloys v Biographical Notices: Minutes of Meeting, Board of Robert Bell, by F. D. Adams. xlix Directors xvii H. J. Cantwell, by H. A. Members in Military Service xviii Wheeler 1 Personal xxiii Institute Committees Iii Employment xxv Officers and Directors Ix

Jan 11, 1917

By T. J. Fabiniak, R. A. Dodd, R. Balow

ALTHOUGH the (111) slip direction in pure bcc metals is well established, the information on operative slip planes is less unambiguously interpreted. So far, (110) {112), and (123) slip planes have been identified, but it is not certain whether glide on (112) and (123) really occurs or if it is composite slip on non-parallel (110) planes. The second of these possibilities is supported by the work of Chen and Maddin on niobium and molybdenum, and a subsequent analysis by these same workers of slip in bcc metals generally.3 The alternative possibility is exemplified by the work of Opinsky and smoluchowsky4 who concluded that slip in Fe-Si crystals can occur on any one of the systems {110}(111), {112}(111), and {123)(111), depending on which system the resolved shear stress is highest. Allen et alS5 also found that glide in ar iron could occur on any of these three systems, the operative system being determined principally by orientation. By an analysis of crystal rotation, slip lines, and X-ray asterism Harris6 concluded that niobium also deforms on these same systems, but if one of these glide planes does not coincide with the plane of maximum resolved shear stress, composite slip on nonparallel (110) planes may occur giving a macroscopic high indices slip plane. Earlier work on iron by Vogel and Brick reached the same conclusion.7 The analysis of slip in bcc metals is made more difficult by the fact that the slip lines may be quite wavy. In fact, the generality of wavy slip lines suggests that screw dislocations slip readily from one plane to another in the (111) zone ("pencil glide") although, as noted, it is not certain whether planes other than (110) really contribute to the slip. If planes of higher indices than {110} do operate, there is a possibility they may do so more readily at higher temperature Argon and Maloof9 observed {100}{211}(111) slip in tungsten single crystals plastically strained at low temperatures, but the results were interpreted in terms of an orientation-dependence rather than temperature-dependence. Therefore, at the present time corroborative evidence for the operation of higher indices slip planes at higher temperatures is lacking. The present results were obtained during the course of an investigation into the effect of cathode and anode surface crystallography on the prebreakdown currents of vacuum insulated devices. In the experiment of particular interest, the 1/8-in.-diam anode and the in.-diam cathode were tungsten crystals (total impurities -230 ppm) with (110) and (100) faces respectively. The faces were electrolytically planed and examined for initial perfection by plastic/carbon replicas and a study of Kikuchi lines in reflection electron diffraction patterns. They were aligned precisely parallel in an insulating holder incorporated into the electron microscope, the measured microscope vacuum being 2 x 10-5 torr, and the electrode spacing 0.01524 cm. The anode structure shown in Fig. 1 was obtained

Jan 1, 1970

United Engineering Society J VIPOND DAVIES,-President WILLIAM L SAUNDERS ALFRED D FLINN Secretary GEORGE H PEGRAM, 2d Vice-president JOSEPH STRUIHERS, Treasurer HENRY A LARDNER Assistant treasurer Finance Committee House Committee WILLIAM L SAUNDERS, Chairman ALFRED D FLINN, Chairman GEORGE H PEGRAMO FREDERICK F SHARPLESS ARTHUR S DWIGHT JOHN H DUNLAP BANCROFT GHERARDI CALVIN W RICE I VIPOND DAVIES, ex-officio F L HUTCHINSON

Jan 1, 1923

By C. Richard Tinsley

INTRODUCTION Project financing has been defined by various authors in this book. It is founded on reliance upon the project's own future cash flows and secondarily on the collateral value of the asset base developed. It is chiefly provided by the banking community who, after an assessment of the risks involved (See Chapter 9) analyse the company's presentation (See Chapter 10) in order to structure a financing package often at a leverage of up to 80% debt. This paper describes the various support and structuring techniques used to delimit and abate the risk components perceived from the banks' experience on project development especially for the period before cash flow is generated (pre completion). ADVANTAGES The advantages of project financing extend beyond the offloading of risks to banks. Among the advantages are the following: 1. Longer loan maturity than conventional, unsecured financing; 2. Loan disbursement and repayment tailored to specific mine; 3. Ability of a joint venture without a "track record" to raise financing; 4. Obtain financing where further direct borrowing (corporate credit) limited by existing indentures; 5. Possibility of arranging finance off-balance sheets; 6. Leverage return on equity; 7. Obtain tax savings with certain project financing structures; and 8. Obtain flexible loan repayment conditions. It can also be said that from the point of view of the company, project financing has certain disadvantages which can be summarised as follows: 1. Perceived higher cost (risk premium) compared with straight corporate credit; 2. More documentation; and 3. Need to negotiate risk-sharing aspects. The main attraction of project financing is the ability to pass certain risks on to the lenders within a flexibly funded transaction. (For a more detailed description of the specific risks see the author's paper at the beginning of Chapter 9. The same risk system is followed here.) The typical project financing has corporate support prior to completion and will usually carefully control the resultant cashflow after completion to ensure the bank does not unnecessarily assume further risks of an equity nature. WITHIN THE COMPANY'S CONTROL Operating Risk This is broken into three interrelated segments for ease of description. Technical Component: This must be specifically addressed if new technology or unproven adaptations are to be used. The banks will have scrutinized the sampling and bulk testing work, perhaps grilling the geological, mineral processing, metallurgical, and mining engineering staff or consultants directly. A number of supports are available such as: TECHNOLOGY GUARANTEE: Either the company itself or the process developer will guarantee that the technology will work for a period of, say, six months to two years after startup. If not, then financial penalties will apply although these are rarely sufficient to repay the loan. Many process developers are weak financially and may have little substance to back such a guarantee.

Jan 1, 1985

By Donald E. Meyer

High current-low voltage EB-gun evaporation in an oil-free ultra-high vacuum system was found to be necessary, though not sufficient, for stability (300°C, 106 v per on) of aluminium gate MOSFET's and MOS capacitors not stabilized by a phosphorous glaze. five characteristics of the equipment used: 1) Vacuum purification of the aluminum charge, 2) Ionization of the evaporant by the electron beam, 3) X-ray formation, 4) Residual gases during evaporation, and 5) Metal film structure were studied as Possibly significant in MOS fabrication. EVAPORATION of contact metals common to the semiconductor industry historically has been accomplished with oil diffusion pump systems and various resistance heated evaporant sources as dictated by the type of metal evaporated. To meet a need for greater reliability of semiconductor devices, other metallization methods were developed. A good example would be application of the moly-gold contact system to integrated circuits with deposition by RF or triode sputtering.' More recently, fabrication of stable metal-oxide-silicon devices and circuits has put new demands on metallization. The purity of the thin metal films composing MOS structures is critical, particularly at the metal-oxide interface, and ultra-high vacuum metallization using sputter-ion pumping and electron beam gun (EB-gun) evaporation are well suited for the task. At this laboratory aluminum has been the most common contact-gate metal for both MOS capacitors and MOSFET's. In the earliest work with MOS capacitors, aluminum was evaporated from wetted tungsten filaments using both diffusion pump and ion pump vacuum systems. In spite of clean oxide techniques these capacitors were unstable under bias-tempera-ture stressing. Only after a switch to EB evaporation of aluminum were stable capacitors produced. Using the same techniques it was possible to make MOSFET's with equivalent stability. Stability data for a discrete MOSFET is shown in Fig. 1. This is a "clean" oxide gate (no phosphorus stabilization or no etch back of a thicker gate) having a thickness of lOOO? thermally grown on the (111) plane. Gate length after diffusion was 0.24 mils, and the devices were hermetically sealed. Stressing conditions were 300°C and 106 v per cm applied alternately as a positive and negative field for 10 min, 50 min, and 4 hr for a total stress time of 10 hr. An initial shift in turn-on voltage of 0.1 v was detected for 10 min of positive bias. All evidence at this laboratory indicated that while EB-gun evaporation of ultra-high purity aluminum was not sufficient for 300°C stability, it did seem to be necessary. There may well then be something inherent in the EB-gun deposition used which enhanced stability, and probably no single factor existed but rather a series of factors. It is the purpose of this paper to report on some of the investigations carried out to learn more about EB-gun evaporation in ultra-high vacuum systems. EXPERIMENTAL DESCRIPTION The EB-gun was self accelerated, had a maximum power rating of 10 kw, and used a water-cooled copper crucible able to hold a 20-g aluminum charge. The electron beam was bent 180 deg and focused by an electromagnet which also provided movement of the beam across the crucible. Normal power conditions in this work were 9 kv and 300 to 600 mamp. The gun can be described as high-cur rent/low-voltage and was quite different in its mechanism of operation from EB-guns with much higher acceleration potentials. An oil-free vacuum system capable of 5 x 10- l0torr, a quartz crystal rate and thickness monitor and a quadruple mass spectrometer completed the evaporation system, Fig. 2. A typical evaporation cycle consisted of a 3 to 4 hr pumpdown to the upper l0-9 range and evaporation at l0? per sec with the pressure in the bell jar not rising above 1 x 10"7 torr. Thickness control was 5 pct or less and could be automatically monitored and controlled. Five phenomena associated with the EB evaporation and considered as possible contributors to Ma performance included a purification effect, ionization of evaporating aluminum, X-rays, constitution of vacuum ambient during evaporation, and film structure dependence upon evaporation rate. These phenomena are now discussed. Vacuum Purification. The design of the EB-gun permitted purification of the aluminum charge by vacuum outgassing. Particular features included an efficiently water-cooled copper hearth with a capacity of over 20 g of aluminum and the capability for sweeping the beam across the charge. Such capacity meant that aluminum had to be added only after about every fifth evaporation. A new charge was not required each evaporation as is necessary with filament evaporation. An oxide "scum" which appeared on the charge could be completely cleared from the top hemisphere of the charge by sweeping with the beam prior to opening the shutter. An indication of the purifying effect was obtained by a series of analytical measurements on incoming aluminum, after melting but with little vacuum out-gassing, after 30 min outgassing, and the evaporated film itself. Either a solids (spark source) mass spectrometer or an emission spectrometer were used for analyzing the aluminum charge. Analysis of the evapo-

Jan 1, 1970

By M. M. Wong, D. E. Couch, G. M. Martinez

The Bureau of Mines electrowon hafnium metal with an average oxygen content of' 150 ppm at 700°C from an electrolyte containing 27 wt pct LiCl, 62 wt pct RbCl, and 11 wt pct HfC14. The average anode and cathode current efficiencies were 90 pct at anode and initial cathode current densities of 86 amp per sq ft. Haf-nium metal with an average oxygen content of 440 ppm was electrowon at 800oC from an electrolyte containing 90 wt pct KC1 and 10 wt pct HfCl4. The average anode and cathode current efficiencies were similar to those obtained in the LiCL-RbCl-HfCl, electrolyte. The chlorine gas given off at the graphite anode was vented through either a silica or a graphite tube to prevent cell corrosion. THE current method for the commercial production of high-purity hafnium is the thermal decomposition of Hfl4.1 The iodide method is not adaptable to continuous process techniques. Nettle, Hiegel, and Baker2 studied the electrorefining of hafnium from hafnium sponge containing 800 ppm oxygen. They failed to obtain hafnium with 600 ppm oxygen in their initial deposits and obtained AEC specification for oxygen only after 75 pct of the soluble hafnium had been removed from the electrolyte. Calculations using their data indicated this was approximately 4 lb of hafnium. The electrolyte was then used to produce approximately 3 lb of hafnium with a low oxygen content. However, no data are shown concerning the amount of anode material initially used or what percent of it was dissolved, therefore, results are not suitable for evaluation of a continuous operation. In general, it was not possible to consistently obtain low oxygen content metal with the electrolytes described by Nettle, Hiegel, and Baker. Wong, Hiegel, and Martinez3 investigated the electrorefining process for hafnium and showed that even by strict control of electrolyte composition only relatively low oxygen reduction could be obtained. The oxygen contained in the hafnium anode material tended to transfer to the cathode deposit and only a limited purification was possible. Both the "iodide" and the "electrorefining" processes depend upon hafnium sponge as a starting material. The sponge is normally produced by magnesium reduction of HfC14 ' and does not meet AEC specifications for hafnium metal. Since only 30 pct of the anode feed could be utilized3 in the electrorefining cells, the Bureau of Mines developed an electrowinning process. HfC14 was used as the feed material for the electro-winning process described in this report. Many of the electrolytes used in the electrorefining studies3 ap- peared to be suitable carrier-electrolytes for HfC14. However, in the initial studies on electrowinning, it was desirable to use electrolytes that had low solidus temperatures and could be operated over a wide temperature range to investigate parameters of the process. Therefore, electrolytes containing LiC1, NaC1, KC1, RbC1, CsC1, and HfC14, in various combinations were explored. EQUIPMENT Chlorinator. Hafnium carbide was chlorinated to produce HfC14 in the batch-type chlorination shown in Fig. 1. Chlorination temperatures were measured with a thermocouple placed in the center of the HfC charge. A flow meter was used to monitor the helium and chlorine. The exhaust side of the silica chlorina-tor tube was equipped with a flask for collecting organic material released during the initial heating of the HfC. The temperature of an internal heater, which extended from the HfC14 condensing flask to the hot end of the chlorinator, was adjusted to prevent the HfC14 from condensing before entering the collection flask. Helium and excess chlorine were exhausted through the lid of the collection flask to an aqueous NaOH solution. Sublimer. Initial studies were conducted using a sublimer, Fig. 2, made by placing a 13/8-in. OD nickel thimble 11 in. long, inside a 11/2-in. ID nickel bell 12 in. long, and locking it in place. This unit was loaded with HfC14 and partially immersed in the molten electrolyte for sublimation directly into the electrolyte. In another sublimer shown in Fig. 3, the HfC14 was contained in a "resin reaction flask". Quartz wool, previously heated to 600aC, secured between two nickel wire screens, was placed just above the HfC14 powder. The lid contained a vacuum outlet, a gage, an argon inlet, and an air-cooled pipe for condensing the HfC14. This sublimer was evacuated and heated. The sublimation temperature was not critical and the sublimer operated satisfactorily at all temperatures between 250" and 350°C. Electrolytic Cell. The electrolyte chamber, Fig. 4, was made of mild steel 8-in. schedule 20 pipe, 30 in. long. The exterior was metallized with a Ni-Cr alloy. The electrolytes were contained in a 16 gage nickel or iron liner with a nickel heat shield on top. The cell was heated by a resistance furnace. A 21/2-in. ID by 25 in. long air lock was connected to one port of a two-port cell cover assembly through a slide valve. The cover assembly of the air lock was electrically insulated from the cell and was equipped with a rubber sleeve that provided for the passage of the cathode lead. This allowed the cathode deposits to be removed and a new nickel cathode to be introduced without allowing air to enter the cell. A tube-rod assembly was bolted to the other port on the cell cover assembly and was sealed by a packing seal. The tube-rod assembly consists of a graphite

Jan 1, 1970

By I. P. Pardee

In our mixture at Musconetcong Iron Works we have an exceedingly hard, dense, magnetic ore, which contains some iron pyrites. The sulphur runs from 0.5 to 1.5 per cent. To prepare this ore better for the furnace, and with a view of making a softer iron, we tried roasting the ore in a Gjers kiln. When it worked well, the improvement in the iron was very perceptible ; but the ore was continually sintering and forming scaffolds across the bosh of the kiln.

Jan 1, 1887

By Konrad Stern

The terms asphalt and bitumen have been applied interchangeably, although incorrectly on occasion, for centuries to various bituminous materials that were found in nature. Native bituminous materials of only the solid types, deposits of which are found on or near the surface of the ground, together with the principal asphaltic type petroleum bitumens will be considered in this chapter. The international dictionary compiled by the "Permanent International Association of Road Congresses" still gives the full name as "Asphaltic Bitumen" but of recent years the word "Bitumen" has been recognized as most appropriate and is defined by the American Society for Testing Materials as follows: "Mixtures of hydrocarbons of natural or pyrogenous origin, or combinations of both, frequently accompanied by their nonmetallic derivatives, which may be gaseous, liquid, semisolid or solid and which are completely soluble in carbon disulfide." Asphaltic pyrobitumens, as defined by Abraham,2 is a species of pyrobitumen, including dark-colored, comparatively hard and nonvolatile solids; composed of hydrocarbons, substantially free from oxygenated bodies; sometimes associated with mineral matter, the nonmineral constituents being infusible and largely insoluble in carbon disulfide. Deposits of native bituminous materials are found scattered over the entire world, but many are relatively unimportant as far as commerce is concerned. No attempt has been made to cover all of the known deposits. The principal bituminous materials of commercial interest are: 1. Native asphalts, solid or semisolid, associated with mineral matter such as Trinidad Lake asphalt, Rock asphalt and Selenitza, Boeton and Iraq asphalts. 2. Native Asphaltites, such as gilsonite, grahamite and glance pitch, conspicuous by their hardness, brittleness and comparatively high softening point. 3. Asphaltic bitumens obtained from nonasphaltic, semi-asphaltic and asphaltic crude petroleum by distillation, blowing with air and the cracking of residual oils. 4. Asphaltic pyrobitumens of which wurtzilite and elaterite are of chief interest industrially as they depolymerize upon heating, becoming fusible and soluble in contrast to their original properties in these respects.2 5. Mineral waxes, such as ozokerite, characterized by their high crystallizable paraffine content. Native Lake Asphalt At Brighton situated in the southwestern part of the Island of Trinidad is one of the largest deposits of native asphalt in the world.3 The lake is oval in shape, covering an area of 114 acres and having a depth of 285 ft at its center. The material forming this deposit is an emulsion of water and bitumen with a suspension of mineral matter consisting of impalpably fine clay dispersed by nature in the asphalt, and small quantities of silica and vegetable matter. The entire mass of asphalt is in slow but constant motion as evidenced by the migration of islands of vegetation from one place to an-

Jan 1, 1960

By C. E. Armantrout, J. A. Rowland, D. F. Walsh

THE close-packed-hexagonal structure of mag-J- nesium is converted to a ductile and malleable body-centered-cubic lattice by the addition of lithium in excess of 10 pct. Further, the density of magnesium or magnesium-base alloys is decreased by additions of lithium. The practical possibilities of such alloys as a basis for uniquely light, malleable, and ductile structural materials were pointed out by Dean in 1944' and by Hume-Rothery in 1945.2 It was apparent to these investigators, however, that more complex compositions would be required if strengths sufficient for structural applications were to be developed in these alloys. In a search for strengthening additions, various investigators w have examined a number of the ternary and more complex alloys containing magnesium and lithium. An investigation of the fundamental characteristics of these alloys was undertaken by the Bureau of Mines. The investigation was initiated with a study of the magnesium-rich corner of the equilibrium diagram for the ternary system, Mg-Li-Al. The following data from published investigations of Mg-Li-A1 alloys were available: 1—a description of isothermal sections at 20" and 400°C through the Mg-Li-A1 constitution diagram by F. I. Shamrai;' 2—a diagram by P. D. Frost et al." showing approximate phase relationships at 700°F for a number of the Mg-Li-A1 alloys; and 3—diagrams showing the constitution at 500" and 700°F for the Mg-Li-A1 alloy system published by A. Jones et al.' Where compositions and temperatures permit comparison, these diagrams show disagreement. The 700°F isotherms of Frost and Jones differ only in the placement of the phase boundaries. But Sham-rai's 400°C (752°F) isotherm shows a variation in phases as well as in phase boundaries. Although rigid comparison of these different isothermal sections might not be justifiable, it seems impossible to reconcile Shamrai's construction with the isotherms of Frost or Jones. The isothermal sections presented in this paper were prepared to determine compositions which might be suitable for age hardening and to develop the general slope and placement of the various phase boundaries in the magnesium-rich corner of the diagram. Sections at 375", 200°, and 100°C were selected for investigation. In constructing these sections, the solubility of aluminum in magnesium, as reported by W. L. Fink and L. A. Willey Vn 1948, was used at the binary Mg-A1 boundary and the solubility of lithium in magnesium was obtained from the equilibrium diagram for that system as reported by G. F. Sager and B. J. Nelson" in the same year. The solubility of magnesium in lithium was determined experimentally and conforms in general to data reported by P. Saldau and F. Shamrai." Parameters for AlLi and MgI7A1, were taken from American Society for Testing Materials X-ray diffraction data cards. Experimental Procedures Although the isothermal sections presented in this paper are not unusually complex, the experimental techniques involved in their construction are made extremely difficult by the relatively high vapor pressure of lithium and the great chemical activity of both magnesium and lithium. Because of these characteristics, which make precise control of the composition of equilibrium-treated filings practically impossible, the disappearing phase method was used in preference to the parametric method in conjunction with metallographic studies. The alloys used in this investigation were melted and cast in an atmosphere of helium using a tilting-type furnace which enclosed a steel crucible and mold in a single unit. Each portion of the charge (500 to 600 g) was cleaned carefully just before placing it in the crucible; and the charge, crucible, and entire melting apparatus were evacuated and then washed with grade A helium while preheating to approximately 100°C. The alloys were melted and chill cast in an atmosphere of helium. Alloys prepared in this way were relatively free from inclusions and a fluxing treatment was considered unnecessary. The cylindrical ingots obtained were scalped and then reduced 96 pct in area by direct extrusion, yielding % in. diam rod. Sections of the rod, approximately 3 in. long, were given equilibrium heat treatments and then sampled for metallographic examination, X-ray diffraction study, and chemical analysis. The surface of each equilibrium-treated rod was machined to a depth sufficient to insure removal of contaminated material before samples for chemical analysis or X-ray diffraction study were obtained, and all decisions on microstructure were based on the examination of the central portion of the metallographic specimen. All specimens homogenized at 375°C were analyzed after this equilibrium heat treatment. When the composition of an alloy placed it in a critical area of the 200" or 100°C isothermal section, a check chemical analysis was made on a sample taken from the alloy specimen as-heat-treated at the particular temperature. Standard chemical procedures of gravimetric analysis were used in the determination of magnesium and aluminum; lithium, potassium, and sodium were determined by flame photometer methods

Jan 1, 1956

[President MRS. REED W. HYDE 84 Mountain Ave. Summit, N. J. First Vice-President MRS. WILLIAM A. SCHEUCH 37 Trent St. Great Kills, S. I., N. Y. Second Vice-President MRS. RUSSELL B. PAUL 6 Brooklands Bronxville, N. Y. Third Vice-President MRS. JOHN C. BURTON 271 Fox Meadow Rd. Scarsdale, N. Y. Fourth Vice-President MRS. DANIEL C. JACKLING Redwood City R. F. D., Woodside, Calif.]

Jan 1, 1940

The Gooseberry Mine is located 38 krn (24 miles) by road east of Reno, 13 km (8 miles) south of Interstate 80. The mine was originally discovered in 1906 and remained in the control of the Martin family of Fresno, who worked the-property with Mexican ranch hands for 68 years. Westcoast took over the property in 1976 from Apco Oil Corporation. During the time the Martins operated the mine, a 305 m (1,000 ft) inclined shaft was sunk with drifts developed on eight levels exceeding a total of 3,000 m (9,000 ft) in length. It is interesting to note that for over one -half century all development ore was stockpiled. West- coast, the United States mining subsidiary of Home Oil Company Ltd., Calgary, Alberta, completed sinking another vertical shaft to the 396 m (1,300 ft) level. Development work between 122 m and 305 m (400 ft and 1,000 ft) levels has proved the existence of a fine ore body over 300 m (1,000 ft) long. The silver-gold ore grade is fairly consistent in the vertical section, but copper, lead and zinc may show slight increases with depth. Average width of the ore bearing portion of the vein is 2.5 m (8.3 ft). Stoping is by cut-and-fill method. Average silver values within the ore zone have increased from the 152 m (500 ft) level to the 305 m (1,000 ft) level, although the gold values do show some decrease. It is not possible for the geological staff to predict the depth of the ore. However, several years of ore reserves have been proved in the existing mining areas. Important ore minerals are argentite, native gold, and electrum. Trace amounts of galena, chalcopyrite, and sphalerite are associated with the precious metal mineralization. The vein is mainly composed of calcite and quartz. Mine-run underground ore is dumped from the hoisting skip into a coarse ore bin followed by a jaw crusher, an impact crusher, and a 600 mt (650 st) fine ore bin. The mill has a capacity of 317 mt per day (350 st per day). Two-stage grinding is done by a rod mill followed by cyclones with the underflow sent to a ball mill in closed circuit with the cyclones. Cyclone overflow after conditioning receives a primary float in four 1.7 cu m (30 cu ft) cells and a second stage of conditioning ahead of 24 0.8 cu m (30 cu ft) secondary flotation cells. No cleaning stages are used. Flotation tailings are cycloned for a sand-slime separation with the sands used as underground stope fill and the slime portion to tailing dam storage.

Jan 1, 1981