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By E. Klar, A. B. Michael

Differences in the electrical conductivities of copper powder sintered under reducing, selectively oxidizing, and neutral atmospheres are related to impurities in solution or as precipitated oxides. The precipitation of impurities as oxides during sintering in nitrogen is proposed for maximizing the conductivity of sintered copper. Conductivity equations for two-phase systems are summarized. Selected equations are applied to porous sintered copper and composite structures. A recent review of the influence of impurities on the electrical conductivity of copper by Gregory et al.1 emphasized that an impurity in solid solution has a much more pronounced effect on reducing the electrical conductivity than when present partly or wholly as a second phase. When impurities in solid solution can be precipitated as oxides, the copper is purified with respect to these elements and the conductivity is increased. Cast and wrought copper, therefore, frequently contain an intentional residual oxygen concentration to oxidize and precipitate impurities less noble than copper. Copper powders generally also contain impurities which can contribute to a reduction in the electrical conductivity of the sintered material. The most deleterious impurities commonly found in commercial copper powders which markedly decrease the electrical conductivity when in solid solution but which can be precipitated as oxides include iron, tin, antimony, arsenic, cobalt, and nickel. In addition to impurities, porosity in sintered copper also contributes to a reduction in the electrical conductivity. The work reported herein discusses the influence of impurities, sintering atmospheres, and porosity on the electrical conductivity of sintered copper. These are important factors for controlling the electrical conductivity of materials such as sintered copper electrical contacts. Several publications on the electrical conductivity of sintered copper and composite materials with random pores or obstacles have incorrectly considered the conductivity to be proportional to the volume fraction of conducting material. However, analyses and equations have been proposed, the earliest of which is perhaps Lord Raleigh's of 1892,' which more accurately describe the conductivity of two-phase systems. These equations which in many cases allow one to closely estimate the electrical conductivity of porous sintered materials and two-phase composites will be reviewed and related to the measured electrical conductivity of sintered copper, copper-graphite. and Ag-W composites. INFLUENCE OF IMPURITIES AND OXIDIZING, REDUCING, AND NEUTRAL ATMOSPHERES Zone-Melted and Leveled Copper. The electrical conductivities of an electrolytic copper and a lower-purity compacting grade of copper powder after consecutive treatments in reducing or selectively oxidizing atmospheres are compared in Fig. 1. The powder and drillings from the electrolytic copper ingot were melted and solidified in a graphite crucible under hydrogen. The vertical zone leveling technique of multiple passes in opposite directions was used to obtain a uniform distribution of impurities. The electrical conductivity was measured on machined specimens 3 by 0.10 in. diam of the zone-leveled material and after the same specimens were consecutively treated as follows: 1) heating in hydrogen at 1600°F for 3 hr; 2) heating in air in a sealed tube so that 0.04 pct 0 was introduced; heating was started at 1000°F for 1 hr and continued at 1800°F for 8 hr; the stepwise diffusion treatment was used to avoid loss of copper due to evaporation of copper oxide at higher temperatures; and 3) final heating in hydrogen at 1600°F for 3 hr. A L&N Kelvin Bridge, type 4306, and a test fixture with knife edges 2 in. apart were used to measure the room-temperature conductivity with an estimated accuracy of ±0.5 pct. In all cases the conductivity of the electrolytic copper was approximately 100 pct of IACS. The conductivity of the impure copper was 80 pct of IACS both in the cast state and after heating in hydrogen. However, after the heating in air, the conductivity of the impure material was 100 pct IACS. After again heating in hydrogen, the electrical conductivity decreased to 60 pct of IACS. This decrease is attributed both to the dissolution of impurities and observed intergranular cracks due to the phenomenon of hydrogen embrittle-ment in copper. These data show that the electrical conductivity of commercial copper as represented by a compacting type powder can be increased significantly by the precipitation of impurities as oxides through heat treatment in an oxidizing atmosphere. Sintered Copper Powder. A commercial compacting type of copper powder pressed to various densities was sintered either in nitrogen, dissociated ammonia, or dissociated ammonia followed by a selectively oxidizing atmosphere of air in sealed Vycor tubes so that 0.06 pct O was added to the material. The electrical conductivity was measured perpendicular to the pressing direction on as-sintered specimens of approximately 3 by 0.25 by 0.15 in. The fully dense material was obtained by zone melting and leveling

Jan 1, 1969

CHARLES KIRCHHOFF, Chairman. ALBERT SAUVEUR, Vice-Chairman. HERBERT M. BOYLSTON, Secretary, Abbot Bldg., Cambridge, Mass. John Birkinbine, J. Esrey Johnson, Jr., Felix A. Vogel, William H. Blauvelt, William Kelly, Leonard. Waldo, James Gayley, Richard Moldenke, William R. Walker, Henry D. Hibbard, Joseph W. Richards, William R. Webster. Henry M. Howe, E. Gybbon Spilsbury, Frederick W. Wood. Robert W. Hunt, A. A. Stevenson, It will be noted that the various interests of the iron and steel industry are authoritatively represented on this Committee by producers of raw materials (iron ore, coke, and other fuels, refractories, etc.) and of finished materials, by consumers, consulting metallurgists, and educators. The primary duties of the Committee are to secure important papers on iron and steel, to promote their discussion, to organize lively and fruitful meetings, and otherwise to foster the interests of the large number of members of the Institute connected with the iron and steel industry in its many phases. Its success during the past year has been noteworthy. Through its instrumentality many valuable papers were presented at the Cleveland and New York meetings, followed by animated and productive discussions, while the attendance of iron and steel men at both meetings was remarkably large and representative.

Jan 5, 1913

J. E. JOHNSON, JR., New York.-It seems to me that it ought to be somebody's job to tie these notch tests with the reversed-stress tests, because the thing that causes failures in structures, in a great majority of cases, is where the material is stressed repeatedly up somewhere near the elastic limit, and the repetition of that stress seems to bring about what I suppose you may call a growth of crystals and that eventually develops into a break. It seems to me that it would be of the greatest value if there could be a coordination of the results of a shock test of some kind with the reversed-stress test, so that we could be sure that a material that had shock-test resistance would have reversed-stress resistance. H. F. MOORE,* Urbana, Ill.-The question raised by the speaker concerning the correlation of results from impact tests of notched bars with the results of repeated-stress tests is a very complicated one. Impact on a specimen sends energy into the specimen, and if the specimen absorbs this energy without fracturing there must be developed both stress and elongation. A notch in the specimen allows but little elongation to take place before rupture, and develops the ductility of the

Jan 5, 1919

By A. F. Taggart

OLIVER C. RALSTON, Salt Lake City, Utah (communication to, the Secretary*).-This paper has appealed to me as being one of the most lucid, well-connected and complete papers on this subject which has been published. To be sure, the concepts called upon in an explanation of the flotation process by these authors are mostly old ones which have been more or less discussed in previous literature, but they have nevertheless been assembled in a most constructive and suggestive manner. We find a new contribution to flotation theory in the effect of fine particles increasing the viscosity of the interfacial film between a liquid and a gas. This phenomenon has been variously hinted at but never definitely stated in accepted scientific terms. The discussion of "contact angles". is very clear and will doubtless be welcomed by those who have not had the opportunity to investigate the literature on this subject, but it is unfortunate that the "hysteresis of the contact angle," observed by Sulman and reported some years ago, is not mentioned or explained. A few other points need discussion in order to call attention to the fact that, while this paper is the best discussion of the subject which has yet appeared, all of the truth has not yet been told.

Jan 12, 1916

By J. W. Richards

There are two essentially different 'types of case-hardening processes; that using a dry mixture in which the object to be case-hardened is packed and kept for the necessary time at the necessary temperature, and the "liquid" proccss, employing a bath of fused salts into which the object is immersed and which by immediate contact case-hardens the surface of the article. The Shimer process belongs to the second class, and was a war emergency invention. Of the liquid melts used as baths, the most effective and most frequently used are melted potassium cyanide and melted sodium cyanide. These may be used either pure or mixed with salts that reduce the melting point and the percentage of .cyanide present. The use of these baths since 1914 has met many commercial difficulties because of the high price and frequent commercial scarcity of the cyanide salts; at present sodium cyanide has practically entirely displaced potassium cyanide. Another trouble is the danger to the workmen handling the cyanide salts, which are extremely poisonous, and the annoying and poisonous vapors or gases given off in the workshop, unless an effective system of hoods and ventilation is provided, so as to prevent the gases from the baths mixing with the air of the room. Porter W. Shimer, of Easton, Pa., has invented a substitute1 for the bath of melted cyanides which case-hardens with equal or greater facility and effectiveness, gives off no poisonous vapors, and costs for chemicals materially less than the cyanide costs in the previously used baths. The process has been in use over a year in a large American works and the following statement embodies the results of practical experience in the use and operation of the process. The Shimer liquid or melted bath consists of a mixture of easily fusible salts that do not possess case-hardening properties, into which is immersed fresh calcium eyanamid, which imparts to the bath case-hardening properties. The composition of the non-case-hardening salts appears rather immaterial. Good results have been obtained by using a mixture of sodium chloride, calcium chloride, and barium chloride in equal proportions by weight; also a mixture of one part sodium chloride

Jan 1, 1920

By Shiou-Chuan Sun, R. F. Wesner, J. D. Morgan

0. C. Ralston and F. Fraas—Dr. Sun and associates have presented an interesting paper not all of which is comprehended by us. The data assembled measure the deflections of particles in an electrostatic field as a function of a number of independent variables and some dependent variables that are not sharply differentiated. These data are all based on a Johnson type machine of definite, well-described geometry, something not often done in electrostatic separation literature. One new fact brought out by this technique is the effect of coal dust on admixed pyrite and quartz. The effects are opposite in character, as should be expected and we do not agree with the authors that these effects are negligible. Fraas' also used a multiple cell "distribution analyzer" and gives in fig. 5 of his paper a straight line plot with no humps or curves. This is not necessarily at variance with Sun's results because Fraas used a larger gap between electrodes and had no evidence of particles adhering to or dropping off the charged electrode. The section of Sun's paper on effect of surface conductivity contains a speculation that the dielectric constant "represents more or less the electrical conductance of the bulk body instead of the surface of the mineral particles." A simple picture of the meaning of the dielectric constant is that it is the specific inductive capacity of a dielectric when used as the dielectric between the plates of a condenser. It is at once evident that the above speculation confuses capacity with conductance—two definitely independent variables. We ask the authors to state in what group or subdivision their garnet belongs; what method and units were used in calculating the data of col. A, table I and their meaning; what was the temperature of the carrier roll and, finally, has any effort been made to investigate the effects of particle shape on distribution in the electrostatic field? S. B. Hudson—I have read this article with great interest. We have been engaged in research work on the principles of electrostatic separation in this laboratory for some time now, and our findings agree with those of the authors in many respects. The article shows evidence of careful and valuable research in the field of electrostatic separation. A "distribution analyser," very similar to that described in an earlier article by one of the authors," was incorporated in an inclined plate-type electrostatic separator designed and built in the Melbourne University laboratory in 1948 for investigation purposes.22 The actual splitting edges were machined from y! in. per-spex, and the paper hoppers were supported on linen thread immediately below the perspex dividers. These dividers fitted into machined slots in a framework to give accurate Yz-in. spacings. The hoppers (staggered) fed directly into a rack of test tubes, which is supported on a vertical pantograph arrangement. The rack was positioned with guides on the horizontal pantograph stand, and this ensured positive alignment when replacing the rack after making weighings. In later work, when much heavier feed rates were used, of the order of 30 to 40 Ib per in. per hr a rack fitted with rectangular metal containers and similarly aligned was used. Some work was done here on comparing the distributions of minerals when passed separately and when passed as a mixture, and it was found that there was quite an appreciable difference in the two results.= However, in our separator the particles do not pass down the plate in a single layer, and this difference is probably caused by collisions of one mineral particles with the other mineral particles. In most of the investigational work here, the change of the center point of the distribution is measured to establish the effect of a variable, such as voltage. Two minerals (zircon and rutile) have been studied rather exhaustively, and it was found that their distributions are very nearly normal. Owing to the sharpness of the distribution curves, the usual method of obtaining the mean or median was inaccurate, and was not used; instead the mean (also the median), calculated on the assumption of a normal distribution, was used to locate the center point of each distribution and proved satisfactory. The effect of polarity becomes very apparent in the plate-type separator where frictional charges play a very important part when using highly resistive minerals such as zircon. With rutile, a comparatively conductive mineral, polarity of the electrode has little effect. On the other hand, the magnitude of the voltage has a far greater effect on conductive than on resistive minerals. Shiou-Chuan Sun (authors' reply)—Thanks are extended to Drs. Ralston and Fraas for their keen interest in this paper. Their questions concerning coal dust,

Jan 1, 1951

By Shiou-Chuan Sun, R. F. Wesner, J. D. Morgan

0. C. Ralston and F. Fraas—Dr. Sun and associates have presented an interesting paper not all of which is comprehended by us. The data assembled measure the deflections of particles in an electrostatic field as a function of a number of independent variables and some dependent variables that are not sharply differentiated. These data are all based on a Johnson type machine of definite, well-described geometry, something not often done in electrostatic separation literature. One new fact brought out by this technique is the effect of coal dust on admixed pyrite and quartz. The effects are opposite in character, as should be expected and we do not agree with the authors that these effects are negligible. Fraas' also used a multiple cell "distribution analyzer" and gives in fig. 5 of his paper a straight line plot with no humps or curves. This is not necessarily at variance with Sun's results because Fraas used a larger gap between electrodes and had no evidence of particles adhering to or dropping off the charged electrode. The section of Sun's paper on effect of surface conductivity contains a speculation that the dielectric constant "represents more or less the electrical conductance of the bulk body instead of the surface of the mineral particles." A simple picture of the meaning of the dielectric constant is that it is the specific inductive capacity of a dielectric when used as the dielectric between the plates of a condenser. It is at once evident that the above speculation confuses capacity with conductance—two definitely independent variables. We ask the authors to state in what group or subdivision their garnet belongs; what method and units were used in calculating the data of col. A, table I and their meaning; what was the temperature of the carrier roll and, finally, has any effort been made to investigate the effects of particle shape on distribution in the electrostatic field? S. B. Hudson—I have read this article with great interest. We have been engaged in research work on the principles of electrostatic separation in this laboratory for some time now, and our findings agree with those of the authors in many respects. The article shows evidence of careful and valuable research in the field of electrostatic separation. A "distribution analyser," very similar to that described in an earlier article by one of the authors," was incorporated in an inclined plate-type electrostatic separator designed and built in the Melbourne University laboratory in 1948 for investigation purposes.22 The actual splitting edges were machined from y! in. per-spex, and the paper hoppers were supported on linen thread immediately below the perspex dividers. These dividers fitted into machined slots in a framework to give accurate Yz-in. spacings. The hoppers (staggered) fed directly into a rack of test tubes, which is supported on a vertical pantograph arrangement. The rack was positioned with guides on the horizontal pantograph stand, and this ensured positive alignment when replacing the rack after making weighings. In later work, when much heavier feed rates were used, of the order of 30 to 40 Ib per in. per hr a rack fitted with rectangular metal containers and similarly aligned was used. Some work was done here on comparing the distributions of minerals when passed separately and when passed as a mixture, and it was found that there was quite an appreciable difference in the two results.= However, in our separator the particles do not pass down the plate in a single layer, and this difference is probably caused by collisions of one mineral particles with the other mineral particles. In most of the investigational work here, the change of the center point of the distribution is measured to establish the effect of a variable, such as voltage. Two minerals (zircon and rutile) have been studied rather exhaustively, and it was found that their distributions are very nearly normal. Owing to the sharpness of the distribution curves, the usual method of obtaining the mean or median was inaccurate, and was not used; instead the mean (also the median), calculated on the assumption of a normal distribution, was used to locate the center point of each distribution and proved satisfactory. The effect of polarity becomes very apparent in the plate-type separator where frictional charges play a very important part when using highly resistive minerals such as zircon. With rutile, a comparatively conductive mineral, polarity of the electrode has little effect. On the other hand, the magnitude of the voltage has a far greater effect on conductive than on resistive minerals. Shiou-Chuan Sun (authors' reply)—Thanks are extended to Drs. Ralston and Fraas for their keen interest in this paper. Their questions concerning coal dust,

Jan 1, 1951

By Dewey J. Sabin

THE Rio de Canada Honda placer property is situated at an altitude of 5500 ft. above sea level in the San Luis Mountains of the Province of San Luis, Argentina. The mine is reached by 70 km. of fair truck road, from the nearest railway station on the Ferrocarril Buenos Aires al Pacifico. The Pan-American airport at Villa Mercedes, 1.40 km. distant, serves as the most convenient point for shipment of gold. Placer mining in the Rio de Canada Honda dates from the time of the Incas and the present native population depends on the gold washed from this river and the adjacent arroyos as a means of livelihood as did the many generations before them. They dig pits to bedrock where they are not driven out by water, and mine the bedrock gravel by means of tunnels and caves. No timber is available and the ground is supported by rock cribs carefully built with the boulders encountered; or with angular blocks of slate rock taken from quarries on the surface.

Jan 1, 1936

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Jan 1, 1938

By L. W. Page

PrEvious to the introduction of the motor vehicle the broken stone or macadam' road met the conditions of rural horse-drawn traffic better than any other type of road, but under fast motor traffic it has been proved to be quite unsatisfactory, and necessitates high maintenance charges. Such a road depends for its success upon the fact that the rock dust fills the voids between the stones and acts as a cement or binder. Under ideal conditions it should be constructed of rock so suited to the volume and character of horse traffic that only enough fine dust is worn from the stones of which the road is composed to take the place of that carried off by wind and rain; and when these conditions are met, the fine dust resulting from the wear of traffic forms with the stone a smooth, impervious shell, shedding the surface water and protecting the foundation. With increase in the number and speed of motor vehicles, however, it was soon found that the cost of maintenance also increased, until at the present day highway engineers consider the old method of constructing and maintaining broken-stone roads increasingly inadequate, and are introducing every known type of binding material other than rock dust to cement the stone together. Among the most prominent types of products in use are those produced from our various petroleums. That the value of modern methods of road preservation was appreciated in this country much earlier than we have been accustomed to believe is demonstrated by the recent revival of an old patent which was granted to one John Martineau, of Elbridge, N. Y., in 1834. Petroleum had, of course, not been discovered at that time, but he claims as his invention and improvement "The application of tar, turpentine, or any of that class of tenacious, cohesive substances, reduced before use to a fluid state, and that state used as a cement, to apply to, and combine with sand, gravel, pebbles, and pulverized stone, such as is used for a Mc-Adam road, or cobble stone, the interstices of coarser material being in all cases filled,'as well as may be, with sand and gravel and cemented with tar or turpentine, to form the wearing face or surface of streets,

Jan 1, 1915

By E. F. Loiseau

IN a paper on the manufacture of artificial fuel, read at the Philadelphia meeting of February, 1878, I enumerated the difficulties which I had to overcome before succeeding in the mixing of coal-dust and clay, the compressing of the same mixture, and the water-proofing of the lumps. The drying of the lumps, after leaving the press, was the remaining difficulty, and it was expected that a plan devised by Dr. Charles M. Cresson, of Philadelphia, would enable us to dry the fuel as rapidly as it was moulded, and that a continuous production could in that way be obtained. The company was reorganized. The works were purchased by the new company at an assignee's sale, and the oven was modified, according to Dr. Cresson's plan. Anticipating a possible failure, I had prepared a plan by which I expected to be able to demonstrate that anthracite coal dust mixed with pitch, could be manufactured with our present machinery slightly modified ; so that after all, if we were compelled to give up the attempt to make fuel for domestic use, there was a possibility of succeeding in the manufacture of a good steam-fuel. The plan suggested by Dr. Cresson for drying the pressed lumps of coal-dust cemented with clay, did not work as well as we expected. It enabled us to dry more fuel than we did before, but it could not be made to dry more than one-half of the lumps produced by the press. The plan was abandoned, and I was authorized to experiment with coal-dust and coal-tar pitch. The cement which is used in Europe to conglomerate coal-dust is ,usually dry pitch, which is prepared by separating from the tar, at a temperature of 572° Fahrenheit, the volatile matters which it contains. Some manufacturers, however, employ crude tar, others, a rich tar, which has been cleared of 25 per cent. of its volatile substances, by heating it to 392° Fahrenheit. But with common tar very weak fuels are obtained, which do not burn well, and give out a strong smell and a great deal of smoke ; it is also necessary to subject them to a baking process, in order to solidify them, and to eliminate the more volatile of the materials contained. This operation of course requires a special plant, the cost of which increases sensibly the price of manufacture, without counting the products

Jan 1, 1880

By H. H. Wright

In many fields edge water is one of the most important factors governing the production of oil. Possibly this fact is not appreciated by many producers except in so far as it may bring about a loss in production from wells drilled on the flanks of structures. In the light of artificial flooding as practiced in New York and Pennsylvania, and of the beneficial effect of natural water-flooding on many wells and leases in the Mid-Continent and elsewhere, it seems reasonable to suppose that very few phases of the petroleum industry hold greater promise for future benefit than the study and control of the natural water drive. Rate of Water Encroachment The rate of movement of water in artificially flooded areas has been referred to as so many feet per unit of time, usually from an injection well toward surrounding producing wells. This definition is vague when used in reference to the movement of natural edge water, inasmuch as such factors as sand thickness, steepness of dip and horizontal extent arc not considered. In the ultimate analysis, only the vertical component of movement affects the production of oil in the natural drive, and in order to define the rate of water encroachment more exactly, such a term as acre-fect per unit time might be used. Thus, where one well is located to each 10 acres a vertical movement of 5 ft. in the water level in a year would be defined as an encroachment of 50 acre-feet per year, and where one well is located to each 20 acres, as 100 acre-feet per year. Such a definition as this is entirely arbitrary, but it takes into consideration to a certain extent the influence of well spacing, and consequent sand drainage, on the rate of water movement. The rate of movement is considered to be an important function of water encroachment, for it is believed that the efficiency of recovery by natural water flood depends a good deal upon the rate of movement. In general, rapid encroachment is thought to effect a poor recovery because of the differential in favor of the movement of water through a sand body and the consequent tendency to trap oil in the sand. Slow movement, on the contrary, is thought to bring about a partial displace-

Jan 1, 1931

By W. C. Hagel, H. J. Beattie

Seven austenitic alloys of varions base compositions and minor-alloy additions were solution-treated, aged systematically between 1200oand 1800oF, and examined by X-ray and electron metallography. Intragranular preczpitations of µ, Laves, s, ?', Ni3Ti, and x phases were observed as a function of composition and aging time and temperatwre. Phase solubility limits were detevtnitzed within 100Fo intervals. These inter metallic compounds fall into two distinct general classes, and whichever class predomznates depends on base composition. It has become increasingly evident that multicom-ponent austenitic alloys are well characterized by their precipitation processes. Since certain groups of elements act as one, the relationships among these processes are reasonably simple; complete identification of such processes is usually attainable by a systematic aging study with a combination of techniques centered on microscopy and diffraction. Several nickel- and cobalt-base alloys illustrating cellular precipitation and its interaction with general precipitation were reported previously.1 The group of alloys covered in the present paper demonstrates precipitation-hardening reactions involving two distinct classes of intermetallic compounds where the predominating class appears to depend on base composition. This dependency ties in with a crystal-chemistry regularity first observed some twenty years ago by Laves and Wallbaum but never amplified to our knowledge. Results of electron-microscope and X-ray diffraction studies on systematically aged hot-rolled alloys known commercially as S-816, S-590, Rene-41, Incoloy-901, M-308, and M-647 are reported here. Some of these alloys have previously undergone minor-phase analyses by other investiators. Alloy S-816 was investigated by Rosenbaum, Lane and Grant,3 and Weeton and Signorelli.4 Rosenbaum found only CbC in hot-rolled bars. Lane and Grant found CbC and a small amount of M6C in the cast structure and stated that both carbides form during aging, most of the precipitation being CbC. Weeton and Signorelli found CbC, M23C6 and a weak indication of a phase after a slow step-down cooling cycle from 2250°F. Rosenbaum also investigated hot-rolled samples of S-590 and identified CbC and M6C. Preliminary information on Rene-41, gained partly from the present work, was reported by Morris.5 Long-time precipitation phenomena in Incoloy-901 at 1350°Fwere investigated by Clark and Iwanski.B heir raw data re- semble those of our present heat with 0.1 pct B, while their interpretation of these data resembles our interpretation of data from another heat with only 0.001 pct B; they made no statement as to boron content. No previous minor-phase studies of alloys M-308 or M-647 have been reported. EXPERIMENTAL METHODS Table I gives alloy compositions in both weight and atomic percent. Specimens were solution-treated from 1700º to 2200ºF, aged at logarithmic-time intervals up to 1000 hours between 1200 and 1800 F, and examined in accordance with procedures previously described in detail. ' ' Phase extractions were carried out in electrolytic cells containing 800 ml of either 7 pct HC1 in denatured ethanol or 20 pct H3PO4 in water. After electrolysis for 48 hr at 0.1 to 0.2 amp per sq inch, residues were separated by filtration or centrifuging. X-ray powder patterns of residues were recorded on a diffractometer for accuracy and on film for sensitivity. Lattice parameters were calculated by least-squares analyses of indexed sin 8 values, and relative abundances were estimated from intensities of strongest lines of each phase. These phase abundances denote relative amounts with respect to each other rather than to the alloy. Mechanically polished specimens were etched in a freshly mixed solution of 92 pct HC1, 5 pct H2SO4, and 3 pct HNO3. Parlodion replicas for the electron microscope were chromium-shadowed in high vacuum at a glancing angle of 20deg. All electron micrographs are reproduced here with the shadowing source above. The correspondence betweenelectronmicrostructures and phases identified by X-rays was established by a high redundancy of correlation between relative amounts at different stages of aging and examination above and below critical transformation or solubility temperatures. EXPERIMENTAL RESULTS S-816 and S-590—The phases found in S-816 and S-590 after various aging and solutioning treatments are listed in Table 11. These data and the observed

Jan 1, 1962

By R. S. Sherwin

The extractive metallurgy of primary aluminum from its ores is discussed with special attention to the production of alumina from high grade ores by the Bayer process, including differences between American and European practice and a brief description of some processes for lower grade ores and the electrolytic reduction of the oxide to aluminum. METALLIC aluminum is not found in nature, but the oxides, hydroxides, and especially the silicates are plentiful. The estimated percentage of in in the crust of the earth is about 8 pct while that of iron is about 5 pct. By far the larger portion of this is combined with silica in the form of various clay minerals and igneous silicate rocks. From the point of view of extractive metallurgy of aluminum, these are low grade ores while the better qualities of bauxite are the high grade ores. There have been various definitions of bauxite but perhaps the best definition at the present time is that bauxite is a rock or earth commonly used as an ore of aluminum or its salts in which the aluminum is present predominantly as a hydrate or a mixture of hydrates and hydrous oxides. It contains varying amounts of oxides of silicon, iron, and titanium and traces of compounds of some of the less common elements. The silica is mainly combined with alumina as clay or clay minerals which are hydrous aluminum silicates, although a part of it may be present as quartz sand. On the American continents, the alumina is mainly present as gibbsite, Al2O3 . 3H2O, and the same may be said of the best known deposits of the Dutch East Indies and some of the deposits in India. In France and other countries in Europe as well as in Africa, the alumina is present mainly as boeh-mite, A12O3 . H2O, but in some of these deposits it is mixed with minor amounts of gibbsite. Some other deposits, such as those in the islands of Haiti and Jamaica, evidently contain two or more hydrates or hydrous oxides of alumina in varying proportions. Perhaps the main portion of the alumina may be present as gibbsite and boehmite with the proportion between the two varying rather widely. In the silicate minerals, including clay, the alumina is chemically combined with silica and has not been separated satisfactorily by mechanical or physical ore-dressing methods. Low grade bauxites are mixtures of hydrates, usually gibbsite or boehmite, with clay, iron oxides, etc. In some low grade bauxites, it is possible to separate a portion of the gibbsite or boehmite, which may be present as relatively hard and coarse particles, from soft or finely divided clay minerals by log washing or similar methods. This has been applied to the product of some mines or parts of them, but on other ores it is not applicable. In some cases the gibbsite or boehmite is almost as fine and soft and of nearly the same specific gravity as the clay minerals so that washing and gravity separations are not successful. The iron oxide, the clay minerals, and a part of the titanium minerals are often so finely dispersed in the ore that any of the physical mineral separation methods, including separations by gravity, particle size, flotation, and electrostatic or magnetic separation, have not been commercially SUCCESSFUL except on relatively small lots of ore. For these reasons, the only available methods of separation on the general run of ores have been methods which would be classed as chemical rather than physical or mechanical separations. Aluminum oxide can be reduced by carbon at temperatures above 1800°C to form metallic aluminum and aluminum carbide or nitride. The temperature for rapid reduction of aluminum oxide to metallic aluminum is about the boiling point of aluminum and above the temperatures necessary to reduce iron, silicon, and titanium so that the direct reduction of an aluminum ore with carbon will produce an alloy of aluminum, iron, titanium, silicon, etc., which may be mixed with carbides and nitrides. Also a large amount of the reduced aluminum may be lost as a vapor except in the presence of some alloying agent such as copper or other metals. While it is possible to refine such alloys or mixtures so as to produce commercially pure aluminum, the methods which have been found are too expensive for the present market. One direct reduction method which found limited commercial use in Germany during World War II was the direct reduction of a mixture of clay containing very little

Jan 1, 1951

By C. H. Burgess

ON June 5, 1947, Secretary of State George C. Marshall in a speech at Harvard University outlined a plan for the economic recovery of Europe. The plan contemplated that the United States should provide assistance which would enable the European nations better to help themselves and to help each other to reconstitute from their war-torn lands conditions which would make possible decent standards of living.

Jan 1, 1950

By Jr. F. M. Perkins.

Capillary forces play a controlling role in water-drive displacement processes both in laboratory experiments and in actual reservoirs, but their quantitative importance may be quite different in the two cases. Because of the importance of conducting laboratory experiments which are representative of field conditions, it is necessary to understand exactly the role of capillary forces in the displacement process. Though a number of experimental investigations related to this subject are contained in the literature, there appears to be a lack of information pertaining to unsteady-state experiments in water-wet media. This experimental study was conducted to obtain additional laboratory data to clarify further the role of capillary forces in both the macroscopic and microscopic flow of oil and water in porous materials. THEORETICAL CONSlDERATlONS The capillary pressure is defined as the difference in pressure between a continuous oil phase and a continuous water phase in a porous material.' The magnitude of this pressure difference depends on the interfacial curvature and the interfacial tension. The interfacial curvature is determined by the geometry of the pore spaces, the wettability of the rock surfaces, and the quantity of cach phase present. Capillary forces are involved in a water-drive displacement process in that they exert a controlling influence on the microscopic fluid distribution which in turn is reflected in the saturation or macroscopic flow behavior. Microscopic Fluid Distribution Because of the microscopic nature of the displacement of oil by water, it is necessary to consider the flow and the fluid distribution in individual pores. On this microscopic scale the capillary Forces, which act over a distance of one or two sand grain diameters, control the distribution of oil and water under static equilibrium conditions. When an external force is applied to the fluids, such as in a water-injection experiment, the applied forces tend to distort the oil-water interfaces. However, in most fine-grained, water-wet sands, the applied pressure difference across one or two grain diameters is usually several orders of magnitude less than the capillary pressure difference. These con-siderations lead to the theory' that even during flow the capillary forces continue to control the microscopic distribution of oil and water within the pores of a porous material for all practical reservoir and laboratory flow rates. This concept of capillary forces controlling the microscopic distribution of fluids has been substantially verified by other investigators3-7 who have found a lack of dependence of relative permeability and residual oil saturation on rate of fluid injection. Macroscopic Distribution The microscopic influence of capillary forces cannot be observed easily and only the effect on the macroscopic or average saturation can be detected. The saturation, of course, is really the point of interest. During a water flood, large differences in saturation at the flood front cause large capillary pressure gradients. This, in turn, causes water to advance ahead of the flood front thereby reducing the capillary pressure gradient in this region. The result is that in homogeneous porous media capillary pressure gradients tend to cause a diffuse displacement front. At low rates in laboratory columns, the front may extend over the entire column length. When the advancing water first reaches the outflow face of a core, the water, which is the wetting phase, cannot be produced because the pressure in the water just inside the core is lower than the pressure in the oil-filled space around the outflow face. This difference in pressure is equal to the capillary pressure for the water saturation existing at the outflow face. Water, therefore, accumulates at the outflow end of the core which causes a reduction in the capillary pressure. Because the capillary pressure does not vanish except at the residual oil saturation,7,8,9 water will not be produced until the residual oil saturation exists at the outflow face. This entire effect,"' which is called the "boundary effect", results in a region of relatively high water saturation near the outflow face. At low rates of injection in a short column, this region of high water saturation may extend over a considerable portion of the column. The influence of capillary forces on the macroscopic flow of oil and water have been described by Leverett.10 For unidirectional, viscous flow in the absence of gravity segregation, the expression in dimensionless form for the fraction of water in the flowing stream, f, is

Jan 1, 1958

By Louis Moyd

The Concrete Research Division, U.S. Corps of Engineers, has developed a simple procedure for determining the coefficients of linear thermal expansion of rocks by means of resistance wire (SR-4) strain gauges. Gauges are cemented to the surfaces of specimens, which are then brought alternately to temperatures of 35OF and 1350F. Results are accurate to the seventh decimal place. IN the course of investigations of the thermal properties of various rocks proposed for use as aggregates in concrete structures, a relatively rapid method of determining coefficients of linear thermal expansion was required. A method which proved to be satisfactory for this purpose was developed in the petrographic laboratory of the Concrete Research Division, U.S. Corps of Engineers, at Clinton, Miss. The method is based on the fact that strain effects in a specimen can be determined by measuring variations in the resistance of an electrical conductor firmly cemented to the surface of the specimen. Equipment for the determination of strain, electrically, has been developed by the Baldwin-South-wark Division of the Baldwin Locomotive Works in Philadelphia. This equipment includes small strain gauges made of coils of resistance wire bonded between thin sheets of paper (SR-4 gauges), and a portable "Strain Indicator" which records variations in the length of the gauges in microinches per inch. Gauges of this type are now in general use for determinations of various mechanically-induced strains, but their use for the determination of coefficients of thermal expansion appears to be a new application. The advantages of the method are that the test specimens may be relatively small and require only a minor amount of preparation, that a large number of tests can be run at the same time, and that the installation and operation of the equipment is relatively simple. The method and equipment described are now in regular use for determining the coefficients of linear thermal expansion of rock samples submitted to this laboratory. Rocks which have been tested include granites, syenites, gabbros, and other igneous rocks, limestones and dolomitic limestones, sandstones, and quartzites. Specimen Preparation: To standardize the conditions of the tests, the rock specimens are sliced by diamond saw into slabs about 11/2x11/4 in. In the case of bedded or foliated rocks, three oriented slabs are cut from the same specimen, and represent, respectively, a direction in a plane of the bedding or foliation of the rock; a direction along the bedding or foliation and at a right angle to the first; and a direction across the planes of bedding or foliation. One of the large surfaces of each slab is lapped for a few minutes with No. 100 abrasive powder to remove saw scars and irregularities. The slabs are soaked in petroleum ether and then dried in an oven to remove all traces of oil picked up in the sawing

Jan 1, 1951

By Louis Moyd

The Concrete Research Division, U.S. Corps of Engineers, has developed a simple procedure for determining the coefficients of linear thermal expansion of rocks by means of resistance wire (SR-4) strain gauges. Gauges are cemented to the surfaces of specimens, which are then brought alternately to temperatures of 35OF and 1350F. Results are accurate to the seventh decimal place. IN the course of investigations of the thermal properties of various rocks proposed for use as aggregates in concrete structures, a relatively rapid method of determining coefficients of linear thermal expansion was required. A method which proved to be satisfactory for this purpose was developed in the petrographic laboratory of the Concrete Research Division, U.S. Corps of Engineers, at Clinton, Miss. The method is based on the fact that strain effects in a specimen can be determined by measuring variations in the resistance of an electrical conductor firmly cemented to the surface of the specimen. Equipment for the determination of strain, electrically, has been developed by the Baldwin-South-wark Division of the Baldwin Locomotive Works in Philadelphia. This equipment includes small strain gauges made of coils of resistance wire bonded between thin sheets of paper (SR-4 gauges), and a portable "Strain Indicator" which records variations in the length of the gauges in microinches per inch. Gauges of this type are now in general use for determinations of various mechanically-induced strains, but their use for the determination of coefficients of thermal expansion appears to be a new application. The advantages of the method are that the test specimens may be relatively small and require only a minor amount of preparation, that a large number of tests can be run at the same time, and that the installation and operation of the equipment is relatively simple. The method and equipment described are now in regular use for determining the coefficients of linear thermal expansion of rock samples submitted to this laboratory. Rocks which have been tested include granites, syenites, gabbros, and other igneous rocks, limestones and dolomitic limestones, sandstones, and quartzites. Specimen Preparation: To standardize the conditions of the tests, the rock specimens are sliced by diamond saw into slabs about 11/2x11/4 in. In the case of bedded or foliated rocks, three oriented slabs are cut from the same specimen, and represent, respectively, a direction in a plane of the bedding or foliation of the rock; a direction along the bedding or foliation and at a right angle to the first; and a direction across the planes of bedding or foliation. One of the large surfaces of each slab is lapped for a few minutes with No. 100 abrasive powder to remove saw scars and irregularities. The slabs are soaked in petroleum ether and then dried in an oven to remove all traces of oil picked up in the sawing

Jan 1, 1951

By AIME AIME

WHEN Vice-chairman Calvert Townley calls the next meeting of the Executive Board of the American Engineering Council of the Federated American Engineering Societies to order in Washington on Sept. 30, it will be the first meeting in that city for almost a year. It is probable that the Board will decide at this meeting whether future board meetings will be held regularly at the headquarters in Washington or whether the plan of meeting at various engineering centers throughout the country, as has been done during the past year, will be followed. The most important business coming before this .meeting will be the election of a president to succeed Herbert Hoover, who resigned after he became Secre¬tary of Commerce. Nominations to fill this vacancy were ordered 'at the last meeting of the Executive Board, to be reported at the September meeting. Special attention will be given the plans for the engineering assembly, extension of employment service, question of licensing and registration of engineers. The engineering assembly, committee has been appointed, with A. P. Davis as chairman, the other members being Philip N. Moore, L. P. Alford, John C. Hoyt and F. A. Vaughn. This committee will work out detailed plans for an assembly to be held in con¬junction with the annual meeting of the American Engineering Council in, January. Tentative plans provide for a three-day session; one day to be given to special meetings of the executive boards of member organizations and committees of the American Engineering Council; one day to the sessions of the American Engineering Council; and at least one day to discussion of some, special topic.

Jan 1, 1921

By E. C. W. Perryman

The wide grooves formed at the grain boundaries when high purity aluminum is attacked by hydrochloric acid or sodium hydroxide have been attributed by earlier workers to the high energy of the grain boundary material. The effect has been investigated for high-purity AI-Fe alloys with up to 0.055 pct Fe as a function of iron content and heat treatment. It is shown that the explanation given above is untenable, but that the results can be explained on the assumption that iron segregates to the grain boundary in solid solution. IN 1934, Rohrmann¹ showed that aluminum of 99.95 pct purity suffered intercrystalline corrosion when immersed in 10 to 20 pct hydrochloric acid, and that the susceptibility to intercrystalline corrosion depended upon the heat treatment given. The greatest susceptibility was found for specimens quenched from a high temperature (600°C) and the lowest susceptibility for specimens cooled slowly from that temperature. Lacombe and Yannaquis2 have shown that super-pure aluminum (99.9986 pct) annealed at 600°C suffers intercrystalline attack in 10 pct hydrochloric acid and that this attack is intensified by anodic dissolution in the same solution at a current density of 10 milliamperes per sq dm. No difference in extent of intercrystalline attack was found between the 99.993 and 99.986 pct Al, which led the authors to suggest that impurities played only a secondary role in the mechanism of intercrystalline corrosion. It was found, however, that the attack at the grain boundaries depended upon the relative orientation of the grains, large differences in orientation favoring rapid attack. Boundaries where the two neighboring grains were similarly orientated showed high resistance to attack as did boundaries between grains which were in twin relationship. These observations led Lacombe and Yannaquis to suggest that the intercrystalline attack was due to lattice discontinuities present at grain boundaries. Assuming that the grain boundary is a layer three to five atoms thick and has a crystal structure which is a compromise between the two neighboring grains it is clear that the discontinuities will increase with increasing difference in orientation between the neighboring grains and hence the increasing tendency to intercrystalline attack. Roald and Streicher³ investigated the effect of heat treatment of aluminum alloys ranging in purity from 99.2 to 99.998 pct on the corrosion resistance in 20 pct hydrochloric acid and 0.30N sodium hydroxide. They found that in hydrochloric acid the intercrystalline attack appeared to be determined by the type and quantity of impurities present and by the relative orientation of the grains. No difference in the susceptibility to intercrystalline attack was observed between specimens quenched and those furnace cooled, from 575°C. In 0.30N sodium hydroxide some materials exhibited intercrystalline attack, this taking the form of V-notches. Rohrmann¹ offered no explanation for the greater susceptibility to corrosion of material quenched from 600°C. It seems possible that this difference is connected in some way with a different distribution of impurity elements in the quenched and slowly cooled specimens. The fact that Roald and Streicher8 observed no difference between quenched and slowly cooled specimens may possibly be due to differences in either rate of cooling or silicon content or possibly both. Both these would be expected to have an effect on the distribution of impurity elements. Although the rate of cooling used by Rohrmann was slightly more rapid than that used by Roald and Streicher the position cannot be clarified because Rohrmann does not give the silicon content and Roald and Streicher give the silicon contents of only a few of their alloys. That Lacombe and Yannaquis2 found no difference in corrosion behavior attributable to impurities between the two materials they used may be because both were of high purity compared with the aluminum used by Rohrmann.¹ Although they found no difference in the corrosion behavior of their two materials it is possible that the results obtained by Lacombe and Yannaquis may, nevertheless, have been influenced by impurity distribution, since, on the transition lattice theory of grain boundary structure, it would be expected that sparingly soluble impurities would tend to segregate to boundaries where the orientation difference is such that there is a greater density of atomic sites of suitable size to contain them. It was considered worth while, therefore, to examine the corrosion properties of a series of materials of differing impurity content with the objects of confirming the experimental observations made

Jan 1, 1954