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By A. J. Shaler

The subject of the mechanism of sintering has received much attention in the past few years, particularly since the beginning of the series of AIME seminars in powder metallurgy of which this paper introduces the fourth. In the first of these, F. N. Rhines1 brought together and discussed the available experimental data on the sintering of pure metallic powder, and succeeded in bringing to a sharp focus the attention of workers in this field on the established observations which a satisfactory theory must explain. Several other authors3,5,6 have, in the last few years, studied the phenomena that occur when cold metallic powders, loose or in the form of compacts, are first brought to elevated temperatures. Some workers' in the field of friction have recently studied the adhesion of solid metal surfaces when they are brought into close contact. These researches have indicated that several separate mechanisms operate simultaneously, at least during the first part of the sintering process. Some of them have been called transient mechanisms4 because they are in general not absolutely necessary to sintering. Powders may be so prepared and so treated that these transient phenomena do not take place during subsequent sintering. This does not mean, of course, that their industrial and scientific importance is any less than that of the steady-state phenomena. The latter are changes that go on during sintering no matter how the powders are made or treated; they cannot be divorced from sintering. One way to analyze the process of sintering into its component parts is perhaps to distinguish between these transient and steady-state phenomena. Some of the transient phenomena have been studied in the past few years. Huttig3 has shown that, when the temperature of metallic powder is slowly raised, the following events generally occur in order: (1) physically adsorbed gases are desorbed; (2) there is an atomic rearrangement of the surface, a sort of two-dimensional "surface-reciystallization"; (3) there is a breakdown of chemically adsorbed surface compounds; (4) there is a recrystalliza-tion in the volume of the metal. All these changes are shown by Huttig and his coworkers to be completed fairly rapidly at lower temperatures than those generally used in sintering and are therefore not a part of the mechanism whereby the density of a mass of powder continues to change after long heating at an elevated temperature. But the first and third of these changes release gases in quantities which may or may not help to control the steady-state mechanisms, depending on when the voids become isolated from the outside of the compact. Among the phenomena studied by Steinberg and Wulff,8 there is the effect on sintering of residual stresses arising from the pressing operation. They found that the lateral surfaces of a green compact of iron are under a longitudinal residual tension-stress of the order of magnitude of half the yield-point for solid iron. If the outside surface is in tension, the core must be under longitudinal compression. When the compact is heated, the surface residual stress is thermally relieved first, and the compact therefore initially expands in the direction of its axis. This is a transient phenomenon, if for no other reason than the possibility of sintering unpressed powders, as demonstrated by Delisle,9 Libsch, Volterra and Wulff10 and others.1 The subject of recrystallization is dealt with further in a separate section, in view of its prominent place in sintering literature. It, too. is one of these transient phenomena. Among the steady-state parts there may be distinguished the attraction between particles and its consequences, the spheroidization of voids in the compacts, and the densification or swelling of the compact. There is considerable evidence4,7 showing that cold metallic surfaces, when brought to within a few interatomic distances of one another, are attracted to each other by forces of the order of many thousands of pounds per square inch. A calculation, discussed in greater detail in another section, shows that this force changes but slightly when the temperature of the surfaces approaches the melting point. Actual measurements of forces of adhesion of this magnitude have been made by Bradley12 on some nonmetals, but none has yet been made on cold or hot metals. This force is of sufficient magnitude to cause some plastic deformation in powder compacts, as will be shown below. A second force of steady-state nature is due to the surface tension, which probably has the same origin as the force of attraction between surfaces.164 A paper by Udin, Shaler, and Wulff1,3 gives the results of precise direct measurements of its value for solid copper. The demonstration of the tendency for the surface tension to shrink a pore was long ago given by Gibbs.17 He showed that its effect on a curved surface between two phases is equivalent to a pressure perpendicular to that

Jan 1, 1950

By R. S. Pratt

IT is proposed to discuss the materials and furnaces, as well as the melting procedures used in preparing metal for casting billets, bars or cakes for mill fabrication. As far as possible, consideration will be given to the alloys that are commonly made in most brass mills producing strip, tube, rod and wire. RAW MATERIAL The basic raw material for such mills, of course, is copper, which may be obtained in the form of ingots, ingot bars or cathodes. Refinery-cast ingots and ingot bars, which are simply double ingots, are supplied in accordance with A.S.T.M. Specifications as regular electrolytic or fire-refined tough-pitch copper. In the wrought-metal industry, the electrolytic brands have been preferred, although during the war large quantities of fire-refined coppers sufficiently pure to be suitable for all existing requirements were imported from South America. With the exception of Lake copper, most primary fire refined coppers produced in this country have not been considered satisfactory for wrought metal alloys. Cathode copper, which is now widely used instead of ingot copper for alloying, is the electrolytically deposited metal that is normally remelted in the production of electrolytic tough-pitch ingots. It is in the form of rough, flat plates not suitable for processing but quite satisfactory for melting when sheared into suitable sizes. Raw zinc is perhaps the next most important raw material and this is obtained in various grades, depending on the analytical requirements of the alloy to be made. The grades of zinc as outlined in the A.S.T.M. Specifications vary in cost with the amount of impurities-lead, iron, cadmium-and are purchased in such a way as to produce the most economical mixture consistent with the purity required in the alloy. Other virgin metals (lead, tin, aluminum and nickel) are used in varying quantities for making copper alloys. These elements can also be purchased in accordance with the appropriate A.S.T.M. Specifications where available. Also available are a number of special alloys, which are used as deoxidizers or as means of adding relatively small quantities of elements not suitable for adding directly as virgin metal. In this category are such materials as phosphor copper or phosphor tin, silicon copper, manganese copper, cadmium copper, and copper-iron or zinc-iron alloys. Some of these alloys may be purchased on a definite alloy basis or may be produced in the plant itself for its own use. For largely economic reasons, however, a great proportion of the charge to the melting furnaces consists of alloy scrap. In the production of many finished products, as much as 70 or 75 per cent of the metal originally cast may be discarded at various points along the production line. This material eventually finds its way back to the casting shop as mill scrap, overhaul or scalping chips, skeleton scrap, rod turnings, or miscellaneous fabricating scrap. One of the most serious problems in the

Jan 1, 1946

US 4,135,913-Extraction of nickel values from iron-containing nickel sulfide ore, particularly pentlandite or nickeliferous pyrrhotite A mixture of raw ore, roasted ore, or iron powder, and coal as a reductant is heated to a temperature of 800- 1000° C in a nonoxidizing atmosphere to convert the bulk of the iron content to metallic iron while diffusing into the iron the bulk of the nickel, the mixture cooled, and the cool material separated into a magnetic fraction containing most of the nickel and a non-magnetic gangue fraction A Illis arid L S Renzoni, assigned to International Nickel Co, Inc Jan 23, 1979 7 pp (75-21) Filed 10-10-75 (621,343) Priority Canada, 10-27-72 (155,032) Same Canadian 981,910, dated Jan 20, 1976 Same British 1,389,145, dated Apr 3, 1975 US 4,135,917-In the recovery of gallium from a solution obtained by the digestion of bauxite or nepheline in an alkali solution for the production of alumina, the digestion solution is neutralized, the neutralized solution evaporated to an op¬timum caustic alkali concentration and adjusted to a ratio of alkali metal oxide to alumina of above 2, the corrected solu¬tion contacted with a gallium-aluminum alloy, arid high-purity gallium recovered from the solution by electrolysis or cemen¬tation K A Badaliants, et al Jan 23, 1979 6 pp (75-109) Filed 12-19-77 (862,201) Priority USSR, 12-22-76 (2,428,¬006) US 4,135,918-Extraction of copper from copper sulfide ore containing also one or more of the metals iron, nickel, arid cobalt Ore is roasted at a temperature of 750-800° C to expel sulfur, the sulfur-free calcine slurried in water containing a sufficient amount of sulfuric acid to supplement any sulfuric acid formed in situ, the slurry heated at 150-165° C in the presence of a reducing gas to form soluble sulfates of metals other than copper while reducing copper to elemental form, arid the slurry filtered to recover copper solids Any precious metals present in the ore will report with the copper solids V A Ettel, A P Devuyst, R Sridhar, arid C. E O'Neill, as¬signed to International Nickel Co, Inc Jan 23, 1979 5 pp (75-117) Filed 3-2-78 (882,610) Priority Canada, 5-13-77 (278,360)

Jan 1, 1980

By Michael Hoch

The phase diagrams of binary systems of some of the transition elements of Groups IV, V, and VI were used to compute the partial free energies of these elements and the free energy of formation of their Laves-type compounds. From these data, isothermal sections of ternary phase diagrams were calculated and compared with experimental results. DURING the investigation of ternary and quaternary high temperature systems formed by the transition elements of Groups IV, V and VI, the binary phase diagrams for these elements available in the literature were studied. In this study, the free energies of formation of the compounds formed in these binary systems were calculated; these values were then used to determine the general shape of the ternary and quaternary phase diagrams. Above 900°C, the transition elements of Groups IV, V, and VI are all bcc and form only Laves-type compounds in binary systems. The investigation was based on the binary phase diagrams published by Hansen.1 The Cr-Nb system was constructed from the data of Elyutin and Funke.' Several unpublished phase diagrams were taken from Schmidt'sLo and English'sl1 compilations. THE BINARY SYSTEMS valuations of the Thermodynamic Functions. Rostokers evaluated the boundaries of the (a + b) field in Ti-base alloys with a two-constant equation. The authors' interest is mainly in the center of the diagrams; therefore the miscibility gaps in the Zr-Nb, W-Cr, Ta-Zr, Ta-Hf, and Ti-W systems were used to evaluate the thermodynamic behavior of the binary systems. Lumsden's4 Equations 29.2, 32.1, and 33.1, page 287, were used for the excess integral free energy FeX, and for the excess partial free energies Fx and replaces b and b replacesP in Lumsden's notation):

Jan 1, 1962

By Darwin Soler

This chapter will outline the operating procedures at Freeport Kaolin Co.5 kaolin mining operations in Georgia, with emphasis on explaining new techniques recently introduced to reclaim mined-out areas for reforestation. Kaolin is found in the central Georgia area (See Fig. 1) in lenticular, sedimentary deposits of high purity. The beds are Cretaceous in age and vary from 4 to 60 ft in thickness, under a cover of sedimentary overburden ranging from 5 to 150 ft. The kaolin beds contain the mineral kaolinite (a hydrous aluminum silicate) and have a particle-size distribution ranging from about 20µ to the submicron level and averaging about 60% below 2µ. The only contaminants in the deposits are coarse mica, quartz particles, and minor amounts of iron and titanium oxides. These kaolin deposits vary widely in quality from deposit to deposit and also vary within individual deposits. Some of the controlling quality specifications which are determined during exploration are viscosity in water suspension, optical brightness index as measured by reflectance, amenability to bleaching, and particle-size distribution. For this reason, only a small portion of the total kaolin reserves in the Georgia belt are suitable for wet processing for the present markets being served. Kaolin clays are selectively mined by different mechanical methods and are beneficiated by both wet and dry processing to produce a number of products used as fillers and coatings in the paper industry; fillers or additives in the paint, plastic, and rubber industries; and as basic raw materials for the ceramic industry. The State of Georgia is the largest kaolin producer in the United States, with 3,206,454 tons produced in 1966, according to U.S. Bureau of Mines statistics. Freeport Kaolin Co’s processing plant is located in Gordon, Ga., about 20 miles east of Macon, Ga.

Jan 1, 1969

By Robert Hoy

If the reader finds that the basic information in a commodity chapter is insufficient, he can consult the appropriate sources in this chapter to find more detailed or more up-to-date information. In these days, technology develops so rapidly that this 4th edition will be somewhat out of date even by the time it is distributed. A comparison of this edition with the 3rd edition (1960) of Industrial Minerals and Rocks will clearly demonstrate how rapidly the scene changes. One of the best sources of new information, of course, is attendance at technical meetings. For example, the papers presented at the national and sectional meetings of AIME usually discuss new developments in the respective divisions of the society. Frequently this information is available in Preprints. In addition some are printed in Mining Engineering and/or the Transactions of the Society of Mining Engineers of AIME. Furthermore, other professional and trade journals contain articles pertinent to the field. A journal introduced in 1967, Industrial Minerals, published by the Metal Bulletin, Ltd., London, is an excellent source of information. The Mining Journal, Ltd., also in London, publishes a weekly journal, a Mining Magazine (monthly), and a Mining Annual Re- view. The latter covers the field from three aspects: (1) by commodities, (2) through technical developments, and (3) geographically. Other useful magazines and periodicals include Engineering and Mining Journal, Pit and Quarry, Rock Products, and World Mining, all published in the United States. In addition many new books related to industrial minerals have been published since the 3rd edition of Industrial Minerals and Rocks. Most of these, of course, are included in the bibliography of each chapter in this volume. Another excellent information source is the proceedings of the Forum on Geology of Industrial Minerals. This group, which held its 11th annual meeting in 1975, is sponsored by a state geological survey or another mineral agency on a rotational basis. The proceedings have been published by the various sponsors and are available as indicated in Table 1. Two major sources of basic industrial mineral and rock data in the United States, and also a good source for many foreign countries, are the U.S. Geological Survey and the U.S. Bureau of Mines. The two agencies publish many reports and maps on a variety of geo- logical and mining subjects. In addition, each agency has an indexed list of all their publications with a free service announcing new publications. (New Publications of the Geological Survey, U.S. Geological Survey, Washington, D.C. 20242) and New Publications-Bureau of Mines, Publications Distribution Branch, U.S. Bureau of Mines, 4800 Forbes Ave., Pittsburgh, Pa. 15213). The U.S. Bureau of Mines (USBM) publishes annually Minerals Yearbooks which provide statistical data on mineral products including production, consumption, imports and exports, as well as information on new developments. Another very useful USBM series is called Mineral Facts and Problems. Editions were published in 1960, 1965, and 1970. Three other major series of publications by the Bureau are Information Circulars, Reports of Investigations, and Mineral Trade Notes. The latter is particularly good for news of foreign developments. A new Professional Paper No. 820 of the U.S. Geological Survey, 1973, summarizes data on the mineral resources of the entire country. The USGS, in cooperation with USBM, other Federal and various state agencies, has also prepared summary reports on mineral and water resources of given areas which include

Jan 1, 1975

By R. D. Reiswig, J. M. Dickinson

The 0s-Ir equilibrium diagram was determined. The diagram is of the simple peritectic type, with a peritectic temperature of about 2660°C. The solid miscibility gap is narrower than previously reported, the nearly vertical solvus lines occurring at about 42 and 63 wt pct 0s. Widmanstaetten figures resembling martensite in some of the two-phase alloys account for a previously suspected transformation. In view of the long history of use of such alloys, it is surprising that the 0s-Ir equilibrium diagram has not yet been completely determined. The boundaries of the miscibility gap in this system have been estimated to be between 24 and 39 wt pct 0s and 79 and 100 wt pct OS. It has been predicted3 that alloys of ruthenium, osmium, and rhenium with the fcc platinum metals should solidify peritectically in their two-phase regions. The metallographic examination of natural osmiridium alloys has been said4 to indicate, by the presence of a martensitic structure, the existence of a transformation or a phase separation. On the basis of superconducting transition temperature measurements, a 70 at. pct 0s alloy was found5 to be two-phase prior to annealing. EXPERIMENTAL The elemental components used in this work were obtained from several suppliers as sponge. The purities, stated by each supplier to be in excess of 99.8 pct, were confirmed in each case by a semiquantitative spectrographic analysis. The pure components were premelted in an inert-gas tungsten arc furnace with the evolution of some fume, crushed, and pickled for use as alloy melting stock. Upon arc melting to the final compositions, no fume evolution was observed. Because weight losses of the order of 15 mg or less were observed in preparing alloy buttons weighing 15 g, "synthetic analyses" were used in determining the compositions of the alloys. Alloys used in this investigation contained 15, 20, 33, 40, 42, 43, 45, 50, 55, 60, 63, 64, 66, 70, 79, and 80 wt pct 0s. Heat treatments of the alloy buttons and pieces thereof were performed in a previously described6 tungsten tube furnace under pressures of 105 torr or less. It was found that homogenization treatments on the specimens were essential to remove the severe coring which was present, a 3-hr treatment above 2300°C removing all the metallographi-cally visible evidence of coring. Following the various heat treatments, the specimens were "vacuum-quenched" by melting a tungsten fuse wire and allowing them to drop onto a water-cooled copper plate. In a few instances, specimens were quenched into molten tin for comparison, but no difference was apparent. Vacuum-quenched specimens cooled from 2400°C to below a red heat in less than 60 sec. Typical equilibration times varied from 3 hr above 2300°C to 88 hr near 1100°C. The utilization of successively longer equilibration times and the approach to equilibrium from both directions indicated that the times used were sufficient to give a close approach to true equilibrium. Heat-treatment temperatures were measured with a calibrated Leeds and Northrup optical pyrometer through a 0.120-in. lateral sight hole in the tungsten heater tube. It was known that the assumption of black-body conditions inside the 1-in.-diam by 10-in.-long tube was unwarranted. The empirical results of work with thermocouples and melting

Jan 1, 1964

By Louis D. Huntoon

CANADIAN gold production is forging ahead annually and the prospects are that it will continue to do so for many years. Table 1 shows recent annual increases. Production for 1933 will probably reach $70,000,000, and further increases are likely in 1934 and 1935. (Data for November and December, 1932, are estimated throughout this article.) The depression sent many prospectors to the woods so during the last two years many new gold areas have been discovered and are attracting real capital for exploration and development. Several mills came into production in 1932 and mills now under construction will start production in 1933. The offices of mining lawyers are busy. Capital for this new work is obtained from well financed mining companies, syndicates, and individuals who were fortunate enough to invest in the dividend-paying gold mines of the north country in the early days. Prospectors and capital are cooperating. An interest is always retained by the prospector or vender and usually a small amount of real money is given the prospector.

Jan 1, 1933

By E. N. Mazza, H. S. Kalish

The effect of sintering types 302, 3028, and 430 stainless steel powder compacts in hydrogen and dissociated ammonia was investigated. It was found that sintering in dissociated ammonia resulted in as much as 0.5 wt pct increase in the nitrogen content of stainless steel even though the dissociation of the gas was complete. Sintering in hydrogen, on the other hand, reduced the nitrogen content of the stainless steel to less than 0.01 wt pct. In the case of the 302-type stainless steel, the low nitrogen content resulted in a material that was largely ferritic, whereas the high nitrogen content rendered the material fully austenitic. Sintering in dissociated ammonia resulted in lower density, generally lower tensile strength, less ductility, and higher hardness than sintering under equivalent conditions in hydrogen. The reduction of oxides on both stainless steel and iron particles was found to be effected by hydrogen partial pressure in the sintering atmosphere. Compacting pressure was found also to effect oxide reduction during sintering. DISSOCIATED ammonia often is used as a substitute'.' for hydrogen in sintering and in annealing, since economic advantages sometimes can be obtained by such a substitution. In addition, anhydrous ammonia contains very little impurity. Thus, dissociated ammonia gas is very dry whereas tank hydrogen often must be freed of oxygen and water vapor prior to use in many applications. The sintering of stainless steel powder compacts as well as bright annealing is well recognized as requiring a hydrogen atmosphere and for the foregoing reasons dissociated ammonia is frequently substituted. It has generally been overlooked, however, that the nitrogen in dissociated ammonia might have an important effect on the sintering process and on the properties of stainless steel compacts. Considered an inert gas in many applications, nitrogen, on the other hand, is very reactive with cer- tain metals. Dissociated ammonia could not be used for hydriding zirconium or titanium. Nitrogen reacts with columbium, tantalum, chromium, uranium, thorium, and many other active metals. Iron and iron-base alloys are, for the most part, inert in nitrogen but there are many borderline cases. It has been reported that stainless steel stabilized with columbium or titanium should not be sintered in dissociated ammonia.3 olybdenum has been reported as reacting with dissociated ammonia to a minor extent.' Although most of the reactions with iron-base alloys are attributed to the action of un-dissociated ammonia and the action of nascent nitrogen, Uhlig4 showed how readily pure molecular nitrogen reacts with and diffuses into 18-8 stainless steel at 1150°C. He also pointed out how readily nitrogen diffuses out of 18-8 stainless steel when heated in pure dry hydrogen, and these thorough investigations on the subject show that commercial stainless steels are nitrogen-bearing, since they are melted in air. The effects of nitrogen in stainless steel, particularly the 18-8 Cr-Ni type, previously have received considerable attention." In 1926, it was pointed out

Jan 1, 1956

By A. Kaufmann, B. Cullity, G. Bitsianes

T0 determine the bulk of the phase diagram, techniques for melting, thermal analysis, heat treatment, metallography, and X-ray diffraction that have already been described were used.' It proved difficult to get definitive results for most of the alloy system because of the large number of compounds, their high melting points, and their extreme brittle-ness which made metallography difficult. The final phase diagram, essentially as shown in Fig. 1, was issued with considerable trepidation.' The phase relationships at the two ends of the system were defined with satisfactory accuracy. In the central region between U,Si, and USi, there was great uncertainty concerning the melting points and even the composition of the compounds. At the uranium end of the system, it is quite clear that a eutectic exists at about 985 °C and approximately 8 or 9 atomic pct Si. The a-to-8 transformation is not appreciably altered by silicon, but the 8-to-y transformation is raised to about 795°C. There is appreciable solid solubility in y-uranium, as demonstrated by the micrographs of Fig. 2. The occurrence of the E phase was not suspected at first, since the alloys as melted and furnace cooled gave no X-ray diffraction or thermal arrest indication of it. However, suitable metallography revealed a rim around each of the compound particles as shown in Fig. 3. Heat treatment above 600°C revealed that the rim was another phase which formed by peritectoid reaction between uranium and U,Si,. This reaction proceeds slowly and it is difficult to get it to go to completion. Consequently, there is some uncertainty concerning the exact composition of P and the exact peritectoid temperature. On the basis of various metallurgical studies, it was decided that the most probable composition for t was about 23 atomic pct Si. Metallographic examination shows the closest approach to a single phase at this composition. Likewise, density and hardness measurements of heat-treated alloys shown in Figs. 9 and 10 show a change in slope at 23 pct Si. This is revealed most clearly by plotting the difference in hardness or density between chill-cast and heat- treated alloys as shown in Fig. 4. Zachariasen2 was able to index the diffraction lines of P and to determine the arrangement of the atoms in the unit cell. He concluded that the composition must be US. However, it is felt that the metallurgical studies are reliable and that Zachariasen's X-ray work does not furnish positive proof that the P phase exists exactly at the stoichiometric composition U3Si. There are many instances in alloy systems where a phase does not occur at the composition dictated by the molecular structure. It is possible that the chemical analyses used in the present work were subject to some systematic error. This seems unlikely, however, since recent work in several laboratories seems to show excess compound at 25 atomic pct Si.

Jan 1, 1958

By Carlton Beal

This paper presents useful charts for conversion of various viscosimeter units into centipoises and graphically summarizes published investigations of the viscosity of air, water and natural gas at high temperatures and pressures. Where possible, charts and correlations were constructed to cover a range of temperature (60°F. to 300°F.) and pressure (14.7 lb. per sq. in. abs. to 8000 lb. per sq. in. gauge) encountered in oil fields. Correlation charts, for the purpose of predicting crude oil viscosity and solubility behavior at oil field temperatures and pressures, were constructed from an analysis and correlation of 1332 viscosity and solubility observations from 953 crude oil samples taken from 747 oil fields. Of these fields, 501 are in the United States, including 75 in California. Of the 1332 observations, 1215 were viscosity values, including 786 of gas-free crude oil, 351 of oil saturated with gas, and 78 under-saturated with gas at pressures above the bubble point. Results show that crude oil viscosity at various reservoir conditions can be predicted with average deviations varying from 24.2 per cent for gas-free crude oil to as little as 2.7 per cent for undersaturated crude oil "above the bubble point." The solubility of crude oil may be predicted from oil gravity and saturation pressure with an average deviation of 22.0 per cent from observed values. In conclusion, it is shown that the viscosity of a gas and gas-saturated crude oil may be predicted within the accuracy of most reservoir computations. Viscosity is a measure of flow resistance; common units are in centipoises (cp.). The object of this report is to present conversion charts and simplified 'correlation charts showing the viscosity behavior of air, water, gas and crude oil and gas-saturated crude oil under oil field temperatures and pressures, which have been known to be as high as 300°F. and 8000 Ib. per sq. in. gauge under subsurface conditions. The viscosity of a liquid or gas is important because it is a measure of its fluidity, or its ability to flow through pipe lines or oil sands. Viscosity of air has become important because it is being used in secondaryl,2 recovery projects. The viscosity of natural gas and water at reservoir conditions is useful because they are almost universally associated and produced with crude oil. The viscosity of gas-saturated crude oil at reservoir pressures and tem peratures is of particular value in making estimates of oil reserves3 and rate of oil recovery from flush pools when production decline data are limited. Instruments Used to MeasuRe Viscosity There are many types of viscosimeters,4 and the instruments most commonly used to measure the atmospheric viscosity of liquids at moderate temperatures and their practical working ranges have been deScribed5,6 in detail. Fig. I and Fig. 2 are viscosity conversion charts which have

Jan 1, 1946

By Henry F. Hebley

This paper brings within the compass of one comparatively brief article a general description of the situation concerning the nation's water resources. It touches upon the phenomenal growth in the demand for water supply and emphasizes the problems facing the coal industry both with regard to acid mine water drainage discharged from active and abandoned mines and the suspended solids discharged to the stream system from wet coal preparation plants. IT must always be remembered, with regard to the problem of water-borne industrial wastes, that stream pollution from any cause is just one factor in the comprehensive problem of water supply in modern times. Industries nonexistent 25 years ago are now flourishing, and supplies of water piped to homes and apartments, as well as the greater number of plumbing fixtures per dwelling and per building, have created an ever growing demand on the country's water resources. Indication of this rapid growth in demand is shown in Table I, which is quoted from Abrams. of Texas increased 287% and the water consumption 7000 per cent." The domestic load varies greatly, depending on the extent of the available supply and the habits of the community. According to the report of the President's Water Resources Policy Commission' the United States Public Health Service reported a national average of 127 gal per capita per day, varying from 60 gal in communities of 500 persons to 140 or 150 gal in cities of 10,000 or over. Other critical areas may be cited to illustrate the inter-relation between new industrial processes and the demands for water in the area where the new enterprise is located. Powell and Wilson have pointed out that during World War 11, in the vicinity of Louisville, Ky., a rapid expansion of industry took place, consisting of numerous synthetic rubber plants. The demand for water increased from 37 million gal per day in 1937 to 62 million gal in 1943. These heavy requirements drew down the supply stored in the water-bearing aquifers to such an extent that urgent plans for recharging were considered. Similar situations have developed in the Los Angeles area and in the vicinity of Texas City. Warne4 has drawn attention to the situation in Los Angeles area, where in the West Basin the withdrawal of ground water in 1945 was 90,000 acre-ft, almost double the amount of the natural fresh water recharge. The draw down has been so severe that the level of the ground water is now below sea level, and sea water is invading the West Basin aquifers at rates up to 300 ft per year. In the Report of the Engineers Joint Council it is pointed out that in the area of Texas City the ground water table has been critically lowered. In 1930 the daily withdrawal from the water-bearing aquifer was 0.5 million gal. By 1945 the quantity withdrawn

Jan 1, 1954

By Carlton Beal

This paper presents useful charts for conversion of various viscosimeter units into centipoises and graphically summarizes published investigations of the viscosity of air, water and natural gas at high temperatures and pressures. Where possible, charts and correlations were constructed to cover a range of temperature (60°F. to 300°F.) and pressure (14.7 lb. per sq. in. abs. to 8000 lb. per sq. in. gauge) encountered in oil fields. Correlation charts, for the purpose of predicting crude oil viscosity and solubility behavior at oil field temperatures and pressures, were constructed from an analysis and correlation of 1332 viscosity and solubility observations from 953 crude oil samples taken from 747 oil fields. Of these fields, 501 are in the United States, including 75 in California. Of the 1332 observations, 1215 were viscosity values, including 786 of gas-free crude oil, 351 of oil saturated with gas, and 78 under-saturated with gas at pressures above the bubble point. Results show that crude oil viscosity at various reservoir conditions can be predicted with average deviations varying from 24.2 per cent for gas-free crude oil to as little as 2.7 per cent for undersaturated crude oil "above the bubble point." The solubility of crude oil may be predicted from oil gravity and saturation pressure with an average deviation of 22.0 per cent from observed values. In conclusion, it is shown that the viscosity of a gas and gas-saturated crude oil may be predicted within the accuracy of most reservoir computations. Viscosity is a measure of flow resistance; common units are in centipoises (cp.). The object of this report is to present conversion charts and simplified 'correlation charts showing the viscosity behavior of air, water, gas and crude oil and gas-saturated crude oil under oil field temperatures and pressures, which have been known to be as high as 300°F. and 8000 Ib. per sq. in. gauge under subsurface conditions. The viscosity of a liquid or gas is important because it is a measure of its fluidity, or its ability to flow through pipe lines or oil sands. Viscosity of air has become important because it is being used in secondaryl,2 recovery projects. The viscosity of natural gas and water at reservoir conditions is useful because they are almost universally associated and produced with crude oil. The viscosity of gas-saturated crude oil at reservoir pressures and tem peratures is of particular value in making estimates of oil reserves3 and rate of oil recovery from flush pools when production decline data are limited. Instruments Used to MeasuRe Viscosity There are many types of viscosimeters,4 and the instruments most commonly used to measure the atmospheric viscosity of liquids at moderate temperatures and their practical working ranges have been deScribed5,6 in detail. Fig. I and Fig. 2 are viscosity conversion charts which have

Jan 1, 1946

By J. Suiter, H. F. Ryan

H. F. Ryan and J. Suiter (CSIRO)—In this paper the authors have presented "a physical model which has as its central hypothesis the solution strengthening of regions along grain boundaries in the order of tens of angstroms thick", and their calculations have used 40Å as the zhalf-width of this boundary region. Selection of this value by the authors suggests that they were unaware of a number of recent field-ion microscope observations of grain boundary structures (e.g., Refs. 29 and 30). The accompanying figure, Fig. 9, shows a portion of an ion micrograph of a tungsten specimen containing a grain boundary, and the regular arrangement of atoms in various crystal planes in each grain can be seen, except in the boundary zone which is not more than two atom diameters in width. Since it is expected that solute atoms will segregate only to the region where the lattice is disturbed, it would seem that a value of 4Å for the half-width of the boundary region would be more appropriate than the value of 40Å assumed by the authors. If the former value is used in Eq. [8] of their paper to obtain curves showing solute concentration in the grain boundary as a function of temperature, the resulting curves differ significantly from those obtained by the authors. Although there are only relatively slight changes in the regions corresponding to higher temperatures (i.e., grain boundary concentrations of approximately 1 at. pet), at lower temperatures the curves are no longer realistic. For example, the curve corresponding to u = 7000 cal per mole gives a solute grain boundary concentration in excess of 100 pet at a temperature of approximately 360°K, and "flattens out" at a grain boundary concentration of about 300 pet! Similar results are obtained with each of the other curves. Ion microscopy of dilute solid-solution alloys has shown that solute atoms give rise to image points which in most cases are of higher intensity than those of the solvent atoms.31 If the same behavior occurs when the solute atoms are present in much lower concentrations then ion microscopy should provide a sensitive tool for studying the segregation of impurities to the grain boundary regions. Although many grain boundaries in tungsten have been examined after different thermal and mechanical treatments, there has not been, as yet, any systematic study of such segregation. In general the micrographs show no clear indications of marked grain boundary segregation, but occasionally areas are found where the grain boundary contains an appreciable number of image points of high intensity in a very narrow zone, see Fig. 9. If it is assumed that these correspond to impurity atoms then it is possible to estimate the impurity concentration both in the grain boundary and within the body of the grains. Application of this method (to a larger area

Jan 1, 1965

By G. S. Jenkins

The statistics set forth by Professor Mitchell in a proceding paper very carefully brought out the points that indicate that a marked amount of consideration must be given to" the haulage problem to adapt it to local conditions as encountered. Professor Mitchell's paper showed a spread of from 10 tons per man to 50 tons per man on the production crews, which spread can be recognized as entirely too large when one considers that the product is being sold at a price within very close limits. While a portion of this spread may be explained by different methods in cost accounting as to what employees are applicable to the production crew, it cannot all be blamed on an accounting method. A good portion must be explained by the improper application of equipment to the needs incurred by the local conditions. It is in an endeavor to go into this phase that this paper is given. It will be necessary to qualify the points covered in order to keep the subject from becoming too wide in scope. Along this line, conditions will be only those involved in bituminous coal mine practices and only the haulage of coal that is loaded with mobile loading machines in seams 4 ft thick and better. Haulage Methods Employed The Consolidated Coal Co. (Illinois) has been operating on a modernized basis for about 20 yr. By modernized we mean the loading of coal with mobile loading equipment. In review of haulage methods, it must be remembered that the main line electric haulage locomotive has been in service for some 40 or jo years. To augment this main line haulage, the mule did a quite satisfactory job during hand-loading days, but was later replaced by the gathering locomotive, either battery or cable-reel operated. This type of haulage was the method in common use at the time the mechanical loading of coal became of major importance and the success or failure of loading machine installations may be largely accredited to haulage facilities in the early days; that is, in the period around 1930. The Consolidated Coal Co. had its struggle with this problem beginning in about 1927 or 1928. We were somewhat fortunate in that we were already using gathering locomotives powered by storage batteries at the time we introduced mechanical loading. This meant that we did not have to spend as much time training motormen and trip riders as many mines did that utilized only mules for their secondary haulage. This was all advantage, and our efforts could be focused on ways and means of providing adequate car service to the loading machine. Like most operations, we endeavored to gear the car service to the capacity of the machine, with a large crew endeavoring to load the maximum tonnage that the machine would handle. Toward that end our first move was to install switches

Jan 1, 1949

By H. H. Stout

In the early fall of 1925, the writer was conducting, in the Ledoux and Co. laboratory, New York, experiments directed toward ascertaining the effect on its impurity content when cathode copper was subjected to a current of various gases at an elevated temperature below the melting point. The apparatus consisted of a vertical I-in. dia. silica tube about 12 in. long, heated on the outside. The cathodes were broken to pass 3/8-in. mesh, and a current of various different gases was passed up through a 4-in. long column of these loose cathode particles in the vertical tube furnace. Temperature was maintained to 1500º to 1600ºF. and the gas treatments lasted from 3 to 6 hr. The writer observed that whenever reducing gas (H2 or CO) was used, these cathode particles stuck together at points of contact with each other. The cohesion was so marked and tenacious that an examination was made of the fractured surfaces, when cathode particles were broken from the cluster. Crystal growth was always found to have taken place across the surfaces where separate particles were in contact, but only after all oxides, sulphates, etc., had been completely removed. The idea of a possible new process was then conceived and was disclosed to A. M. Smoot (V. P. Ledoux and Co.) with intent to obtain his views. The first conception as given Smoot was "to gas-clean broken cathodes, put them in an extrusion press, solidify and extrude them at around 1500ºF." Smoot's reaction, after a few moments considera- tion, was, "It looks perfectly all right to me.'' The writer and his assistants, W. H. Osborn and H. H. Stout, Jr., after conferring as to ways and means, decided to go ahead with preliminary laboratory experiments, which, it was thought, would move the new process from the possible to the probable. This program followed a course indicated by three basic considerations: 1. Since brittle cathodes were often unintentionally produced, it seemed probable that the laws controlling this type of deposition could be ascertained. 2. We had already proved the gas-cleaning feature. 3. There remained to prove: whether a sound, homogeneous metal billet could be produced with crystal growth established over the entire surface of each individual particle in the billet; and, if so, what would be the physical properties? Osborn arranged with Columbia University for conducting experiments in its research laboratory to prove or disprove the third item; Columbia assigned C. A. Phillipi, Jr. to assist in the project. A press with a cylinder 2 in. high and of I-in. dia. was used. It was surrouilded and heated by a resistance coil 01 Nichrome wire. Broken tough cathodes were used. Experimental Procedure The first run took place March 18, 1926. The resistance wire gave out when temperature of 1000ºF. was obtained. Pressure was immediately applied: perceptible ram movement stopped when 39,000 lb. per sq. in. on the copper was reached, with a maxi-

Jan 1, 1941

By R. N. Orava, L. A. Rice

One of the difficulties encountered in the preparation of titanium specimens for transmission electron microscopy is the formation of a surface hydride phase during the thinning operation at ambient temperatures. This necessarily destroys contrast, obscures features of interest, and often leads to misleading results. By cooling the polishing solution to temperatures below 0°C this problem has been overcome in the past.' However, since the cooling procedure is somewhat inconvenient, a technique was developed at this laboratory for thinning titanium at room temperature. The material examined was A-70 grade commercial-purity titanium purchased from the Crucible Steel Co. of America. The mechanical and thermal treatments, described elsewhere,* yielded a recrystallized grain size of 4 to 5 p. A slice, 0.5 mm thick and 1.5 mm wide, was cut from a bulk specimen2 using a diamond cut-off wheel. The sample was then coated with paraffin wax. Two concentric holes, about 0.03 in. in diam, one at each broad face, were scribed through the wax to the surface of the metal. Subsequent polishing for several minutes resulted in a preferentially thinned or "dimpled" region. Thereafter, the wax was removed and the entire specimen polished to the point of breakthrough at the base of the dimple. Polishing was effected chemically in a solution comprised of 30 pct HF and 70 pct HN03 by volume, kept at room temperature (20" to 25OC). The specimens were mounted in a stereo holder and examined at 100 kv in a Philips l00 B Electron Microscope. A micrograph from a foil prepared in this way is shown in Fig. 1. Several points are noteworthy. This electron micrograph shows neither evidence for the formation of a hydride phase due to specimen preparation nor, moreover, any obvious surface contamination in electron-transparent areas of a freshly prepared foil. Localized variations in foil thickness observed in some specimens seem to be a characteristic of this chemical polish but do not seriously detract from foil quality. With care, the lifetime of a good specimen exceeded 2 hr in the beam. On the other hand, the exposure of a sample to air at atmospheric pressure, when still warm from the beam, clearly resulted in the deterioration of a formerly clean area just previously in the field of view. An example in Fig. 2 of a contaminated region reveals features, and "spots", not unlike those observed in much purer material by Yamane and Ueda. Consequently, one can conclude that: 1) titanium can be thinned satisfactorily in a solution at room temperature for transmission electron microscopy; 2) large-scale precipitates, >50A in diam, are absent in commercial-purity, recrystallized, furnace-cooled, A-70 titanium containing about 3800 wt ppm interstitials and the same amount of iron; 3) care must be taken not to attribute surface contaminants to precipitates. The authors are grateful to the Franklin Institute for financial support and permission to publish.

Jan 1, 1967

By D. H. Baldwin, R. E. Reed-Hill

Six compositions of polycrystalline ZY-0 alloys, containing up to 4.2 at. pct 0, were tested in tension between 77° and 600° K. The data obtained from each of the compositions corresponded closely to a rela-ion between yield stress and absolute temperature of the form In s/so = BT, where oo is the yield stress extrapolated to zero degrees and B is a constant. In agreement with others who have observed this relationship, it is shown that the activation energy may be expressed as Ho In so/s. In the present specimens Ho is approximately 18,000 cal per mole and is apparently independent of temperature and composition inside the limits of the investigation. It is also demonstrated that this form of activation energy cowesponds to a strain rate sensitivity parameter RT/Ho. Oxygen was also noted to have an effect upon the operative deformation mechanisms. With increasing oxygen concentration there was an increased tendency to observe both nonbasal slip and cross-slip phenomena. Oxygen does not seriously inhibit twinning more than it does slip. Twins were observed in all specimens tested. It is becoming increasingly evident that interstitial atoms in solid solution are able to interact strongly with mobile dislocations. Stein, Low, and seybolt,&apos; have shown that, if the carbon concentration in bcc iron is lowered below the solubility limit, its flow stress temperature dependence is markedly reduced. This suggests that carbon atoms in interstitial solid solution may be responsible for the pronounced temperature dependence of the flow stress normally observed in iron. This view has recently been challenged by Leslie and sober2 who observed a strong flow stress temperature dependence in iron to which a trace of titanium had been added in order to remove carbon atoms from solution. Since the interstitial concentration must be reduced below approximately 1 ppm in order to produce a pronounced effect on the flow stress temperature dependence,&apos; studies of the effect of interstitials on the flow stress in iron necessarily involve serious experimental difficulties in alloy preparation. There are other metals, however, in which strong effects of interstitial solutes upon both the flow stress and its temperature dependence are observed. Of particular significance is zirconium which, according to Domagala and Mcpherson, 3 is capable of dissolving 28.6 at. pct O. The O-Zr alloy system is an almost ideal system for studying the interaction of interstitial atoms with deformation modes since it is possible to form alloys capable of study over an extensive range of compositions. Mills has made such a study using single crystals oriented primarily for single prismatic slip4 and has found an effect of oxygen concentration on the flow stress temperature dependence analogous to that observed in iron due to carbon by Stein, Low, and Seybolt. The present paper is specifically concerned with the effect of oxygen on deformation in polycrystalline zirconium. Although plastic flow in this type of specimen is much more complex than that reported for the single-crystal work, and involves both slip (on several different types of planes) and mechanical twinning, the results of this investigation are in general agreement with the single-crystal observations concerning the effect of oxygen on the temperature dependence of the flow stress. In addition, they also demonstrate that oxygen affects the acting deformation systems. This is in contrast to single-crystal results4 that showed only single slip on a prism plane. EXPERIMENTAL PROCEDURE Material. High-purity hot-rolled zirconium strip, 0.2 in. thick by 4 in. wide, of 0.10-mm average grain diameter, was used for forming alloys. It was obtained from the Carborundum Metals Co., Akron, N.Y., whose analysis indicated the major impurities were, in wt ppm: Hf, 540, C, 145; Fe, 100; and 0, <80. The plate texture was similar to a wire texture, with basal planes generally parallel to the rolling direction and basal poles randomly distributed about the rolling direction. The heat treatments described below did not appreciably alter the basic texture. specimen Preparation. Small threaded-end tensile specimens were machined from the plate with axes perpendicular to the rolling direction. These transverse specimens had gage sections 1 in. long by 0.060 in. in diam. The small gage section diameter was dictated by the fact that the alloys were formed by dif-

Jan 1, 1969

By John C. McDonald

This report is a continuation of an earlier one with a similar titlell to which the reader is referred for such details of procedure as do not appear here. A brief summary will be given of the objects and methods of the research at this time. It was pointed out in the previous paper that properties of magnesium alloys, as reported by different workers, often differ. This was thought to be due to differences in the preparation of the specimens tested. The ideal way to compare alloys would be to prepare each of them in so many ways that reasonable assurance would exist that the best properties of each alloy had been developed. The alloys would then be compared on the basis of these properties. The treatment actually given the alloys of these studies is necessarily a compromise with completeness. Nevertheless, enough treatments have been given so that a considerable degree of assurance exists that the properties obtained are representative of the alloy as such, and not merely of the manner in which it was worked and heat-treated. Procedure The alloys were cast in the form of cylindrical ingots, which were extruded into bar before being rolled. Some of the ingots were made in 2-in. diameter molds whereas all of the alloys of the previous paper were cast in 4.in. molds. For the larger ingots, the extruded bar was 2 by 0.140 in.; lor the 2-in. ingots, it was I by 0.100 in. Preliminary work indicated that strip rolled from both sizes of the bars would have substantially the same properties. The bar was rolled at some temperature in the range 400&apos; to 800°F., for a total reduction of 50 per cent. The temperature and reduction per pass were so selected that no cold cracking occurred, but were such as to leave the metal in a semihard condition. The hot-rolled metal was annealed at several temperatures in the range 400&apos; to 800°F.; it was also cold-rolled, and given solution and aging treatments. Two standard test bars corresponding to each treatment were pulled in tension, and the average was obtained. Twelve treatments, in all, were given each alloy. The properties of the annealed specimen having the highest percentage of elongation were selected to represent the alloy in the annealed condition. The properties of the cold-rolled specimen having the highest yield strength were selected to represent the alloy in the cold-rolled condition. These properties were then plotted against percentage composition by analysis. Smooth curves were drawn among the points, thus graphically averaging the results over the entire range studied. The percentage of elongation in the cold-rolled state was not plotted, since it was always low, and varied in an irregular manner with composition. Alloys Studied Magnesium-calcium Alloys.—Fig. I presents the results on the alloys of the rnag-

Jan 1, 1941

By John C. McDonald

This report is a continuation of an earlier one with a similar titlell to which the reader is referred for such details of procedure as do not appear here. A brief summary will be given of the objects and methods of the research at this time. It was pointed out in the previous paper that properties of magnesium alloys, as reported by different workers, often differ. This was thought to be due to differences in the preparation of the specimens tested. The ideal way to compare alloys would be to prepare each of them in so many ways that reasonable assurance would exist that the best properties of each alloy had been developed. The alloys would then be compared on the basis of these properties. The treatment actually given the alloys of these studies is necessarily a compromise with completeness. Nevertheless, enough treatments have been given so that a considerable degree of assurance exists that the properties obtained are representative of the alloy as such, and not merely of the manner in which it was worked and heat-treated. Procedure The alloys were cast in the form of cylindrical ingots, which were extruded into bar before being rolled. Some of the ingots were made in 2-in. diameter molds whereas all of the alloys of the previous paper were cast in 4.in. molds. For the larger ingots, the extruded bar was 2 by 0.140 in.; lor the 2-in. ingots, it was I by 0.100 in. Preliminary work indicated that strip rolled from both sizes of the bars would have substantially the same properties. The bar was rolled at some temperature in the range 400&apos; to 800°F., for a total reduction of 50 per cent. The temperature and reduction per pass were so selected that no cold cracking occurred, but were such as to leave the metal in a semihard condition. The hot-rolled metal was annealed at several temperatures in the range 400&apos; to 800°F.; it was also cold-rolled, and given solution and aging treatments. Two standard test bars corresponding to each treatment were pulled in tension, and the average was obtained. Twelve treatments, in all, were given each alloy. The properties of the annealed specimen having the highest percentage of elongation were selected to represent the alloy in the annealed condition. The properties of the cold-rolled specimen having the highest yield strength were selected to represent the alloy in the cold-rolled condition. These properties were then plotted against percentage composition by analysis. Smooth curves were drawn among the points, thus graphically averaging the results over the entire range studied. The percentage of elongation in the cold-rolled state was not plotted, since it was always low, and varied in an irregular manner with composition. Alloys Studied Magnesium-calcium Alloys.—Fig. I presents the results on the alloys of the rnag-

Jan 1, 1941