Search Documents

By Gerald Edmunds, C. W. Siller, E. A. Anderson

In the pressurc die-casting of zinc alloys it is customary to force the molten alloy under high pressure into a permanent steel die by means of a plunger moving in a bushing that has a clearance on the diameter of the order of 0.002 in. Successful operation of the plunger type of machine requires the presence in the zinc alloy of certain percentages of aluminum. Without these aluminum additions, the normal reaction of molten zinc on ferrous materials causes sticking of the plunger arid a complcte shutdown of the equipment. All of the zinc alloys used for pressure dir-rnsting today contain approximately 4 per cent of aLUminum, which is more than suffieient to make plunger opcration feasible. The clearancc bet,ween the plunger and its bushing is an important matter. As the space bccomes larger, there is a loss in effective metal pressure. Ordinary gray cast iron served fairly well and is still uscd in some machines. However, the rate at which the plunger c1earance. increases with this material is considered by many to be far too great. There is, therefore, a serious interest in finding new matcrinls more: capable of retaining the desired clearance during long periods of use. Today marly die casters are using special materials for plungers and bushings selected by the somewhat expensive and time-consuming test of actual experience. An analysis of the problem reveals two possible end points of plunger. operation: (1) the building up of zinc-alloy plunger-material reaction products in sufficient bulk to cause sticking and (2) rapid solution, wear or erosion, all of which will increase the clearance to an undesirable extent. If neither of these takes place, the pluriger will operatc for a long time, of course.. The authors have developed a laboratory apparat,us in which the action of a plunger moving in a bushing immersed in molten zinc alloy could be simulated closely. Such a machine made possible a more rapid and less expensive survey of the available construction materials and an analysis of the specific alloying reactions taking place in the clearance area.

Jan 1, 1940

By L. E. Murr, P. J. Smith

A study has been made by transmission electron microscopy of thin foils of 304 stainless steel fatigued external to the electron microscope in reversed bending, and of thin foils fatigued directly within the microscope in alternating tension. The build-up of stacking faults in the thin foils during fatigue zoas correlated with the dislocatirm structures found in thin films prepared fror fatigued bulk specimens. The performance of the special devices designed for fatigue of thin foils so outlined and the importance of alternative methods of preparation of more uniform fatigue specimens bY vapor deposition are emphasized. INVESTIGATIONS on fatigued bulk aluminum1,' and stainless stee13j4 have revealed the existence of dislocation substructure on examination by transmission electron microscopy of electrolytically thinned foils representative of these bulk specimens. While this technique has proved extremely valuable, it has several shortcomings. First, the method of fatiguing bulk specimens and then thinning to foil for electron-transmission observation allows only one observation of internal structure at any one portion of the fatigue life. Second, thinning the bulk fatigued specimens to foil results in the loss of at least one original surface. Thus, what one sees in the remaining electron-transparent sections is an internal dislocation or fault structure which in many cases cannot be correlated with the original surface markings. This is an undesirable feature, since it is well-known that metal surfaces play an important part in the fatigue process.5 An obvious third undesirable feature of the thinning-from-bulk technique is the fact that static observations have difficulty (in the case of fatigue) explaining the mechanism of a dynamic process. What is required then is a method whereby a selected thin area can be continuously observed either while undergoing cyclic deformation or at various fixed stages of fatigue deformation. While Murr and wilkov6 have reported some success with an apparatus designed to fatigue thin metal foils directly within the electron microscope, the nature of the specimen-mounting procedure and the mechanical features involved in the adaptation of the fatigue device to the electron microscope make this method difficult to operate. It was not possible, for example, to make frequent observations of a selected area because of difficulty in maintaining a chosen area in a stable viewing position inside the electron microscope. Except for the build-up of a dislocation substructure and what are commonly referred to as "slip striations", little else has been reported from observations on thin-foil sections prepared from bulk fatigue specimens. segal17 has found "slip striations" in stainless-steel fatigued specimens which were electropolished from both sides, but gave no explanation as to their origin or identity in terms of lattice imperfections. The research to be reported in this paper was undertaken with the following objectives in mind. First, an attempt was made to devise a technique or techniques whereby thin metal foils could be fatigued and repeatedly observed by transmission electron microscopy. Second, it was hoped that some correlation could be made between deformation striations found in fatigued thin transmission specimens and thin foils prepared from bulk fatigued specimens. These investigations illustrate quite convincingly that a feasible method is available for the direct study of the fatigue mechanism and similar dynamic phenomena in thin transmission specimens inside the electron microscope. I) EXPERIMENTAL METHODS Three modes of specimen fatigue and observation of fatigue damage were used. These involved fatigue of thin-foil specimens in a special arrangement external to the electron microscope and observation of a selected area at various stages in the fatigue life, the fatigue of thin-foil transmission specimens inside the electron microscope, and the fatigue of bulk specimens external to the electron microscope followed by thin-foil preparation for direct observation at predetermined stages. Design of the External Fatigue Clip and Specimen Holder for the Hitachi H.U.11 Electron Micro-scope. The purpose of the fatigue clip was to provide a reversed bending fatigue stress to a thin-foil transmission specimen outside the electron microscope. In order to accomplish this, a flat-bottomed, U-shaped brass clip was made as shown

Jan 1, 1965

By Jay J. Burns

TWO zinc concentrating mills are operated by the St. Joseph Lead Co. in St. Lawrence County, N. Y. The Edwards mill is operating at present only sixteen hours a day treating 400 tons daily. The metallurgy at Edwards presents no unusual problems therefore this discussion is mainly limited to the metallurgy of the Balmat ore. The Balmat mill has a capacity of 1,250 tons per day and the operating crew consists of three shift bosses each with five millmen per shift. Two crusher operators work on each of two shifts and one cleanup man on day shift. The repair crew is made up of a foreman and three repairmen, one of the repairmen being capable of taking over any operating job in the mill from shift boss down. Each millman is capable of handling the next job in line and several men in the yard crew are broken into handling the start-off job in the mill so that temporary shortages of men do not cause extensive overtime. Sphalerite, pyrite, and galena, the principal ore minerals, occur in a gangue of calcite, dolomite, and silicates, especially diopside, plus tremo-

Jan 1, 1947

By E. J. Ripling, S. I. Liu

IT has been shown in a number of recent publications that much information on the mechanical behavior of metals can be gleaned by first deforming test specimens under one set of conditions, and then evaluating the effect of this deformation by means of a subsequent tensile test. A straining procedure of this type has been applied to study the flow behaviors of a number of metals.1, 2 In these studies the prestraining and testing were both tensile strains, while the straining temperature was varied between the prestraining and testing steps. These data indicate that there is a more or less general flow behavior exhibited by all metals which are pre-stretched at one temperature and then tested in tension at a second temperature. Prestraining a metal at a high temperature produces a lower yield strength during the subsequent low temperature strain than would the same total strain at the lower temperature. On reversing the order of the strains, low temperature prestraining produces a higher yield strength during the subsequent high temperature straining than would a single high temperature strain of the same magnitude. Unlike the flow behaviors, the fracturing characteristics of metals when prestrained under one set of conditions and tested under a second set of conditions is quite material dependent. The fracture behavior of a number of steels2" as well as of a commercially pure zinc,4 have been investigated by these two-step tests and was found to depend upon the position of the transition temperature with respect to the prestraining and testing conditions. Since these fracturing phenomena are complicated by the appearance of the transition temperature, it has been difficult to reliably define the basic effect of a two-step straining procedure in fracturing. Metals crystallizing in the face-centered cubic system do not exhibit transition temperature effects so that the mechanical characteristics obtained on these materials could serve as a base for two-step straining behaviors. Consequently groups of specimens of the aluminum alloy 24s-T4 were prestrained various amounts at room temperature in either tension or compression after which these strained specimens were further strained to failure, or tested in tension, at either room or some lower temperature. Other groups of 24S-T4 specimens were prestretched at various low temperatures after which these were tested in tension at room temperature. These straining techniques then made it possible to compare the behaviors of aluminum with the behaviors previously presented for steels. Material and Procedure The commercial aluminum alloy 24S-T4 in the form of 3/4 in. rods was used in this investigation. The material was subjected to the following treatments before machining: 1—resolution treating at 920" & 10°F for 45 min, 2—quenching in water at room temperature, and 3—aging at room temperature for four days. The re-heat treated material was then machined to either of the specimen shapes shown in Fig. 1. Fig. la shows the threaded-end specimen used for prestraining in compression. Fig. 1b shows the specimen used for both prestrain in tension and final testing. The material subjected to precompression in the form of the specimen shown in Fig. la was re-machined to the specimen shape in Fig. 1b for final testing. Prestraining in tension and final testing were done without any intermediate machining. All straining was performed on a 10,000 1b Riehle tensile testing machine. Tensile strains were conducted in a specially designed concentric fixture which produced an eccentricity of less than 0.001 in." The change in diameter at the minimum section of

Jan 1, 1954

By A. W. D. Hills, M. R. Moore

An apparatus has been developed in which metals can bc solidified under closely controlled unidirectional heat flow conditions. The metals are cooled by a multiple-air jet system, designed so that the heat transfer coefficient is uniformly distributed over the cooled surface. They are contained in a special furnace system of low thermal mass which enables unidirectional heat flow conditions to be rigorously maintained for certain specific cooling rates. This apparatus has been used to study the solidijication of pure lead and pure tin at zero superheat, solid metal thicknesses being determined by thermal analysis, and by dipstick readings. Detailed thermal balances have been drawn up on the experiments in order to determzne the cooling conditions that most rigorously correspond to unidirectional heat flow. Solid metal thicknesses, measured experimentally for these conditions, have beetz shown to agree closely with the theoretical wedictzons of different integml-profile methods. lt is concluded that any errors inherent in the integval-profile method are no greater than the errors inherent in experimental investigations of solidification. A knowledge of the influence of heat transfer rates on the solidification of metals is essential to the understanding and control of industrial casting processes. Since very few formal methods are available for solving the heat conduction equation under solidification conditions several authors have developed approximate techniques for doing so. One of the most promising is the integral-profile technique that has been used by Goodman,1 Hills,2,3 Tien4 and Hills and ~oore' to predict solidification rates under certain specific heat transfer coniditions. In the first of this present series of papers6 Hills has further generalized the method and developed a universal integral-profile technique that can be used to predict solidification rates under a wide variety of unidirectional heat flow conditions. Since the method is approximate it is necessary to investigate the accuracy with which it predicts actual solidification rates. A review of the literature7 shows that solidification rates have seldom been measured under accurately known heat transfer conditions and it was therefore decided to develop experimental techniques that would enable this to be done. Results obtained would then be available as a check on the approximate solutions already developed, and in the development of further solutions that would be applicable under more complicated conditions. The initial work in this experimental program which is described here, is concerned with the solidification of pure metals at zero superheat under unidirectional heat flow conditions. Subsequent experiments have been concerned with the solidification of pure metals at appreciable superheats, under varying unidirectional heat flow conditions and under two dimensional heat flow conditions. In a series of experiments recently initiated, the solidification of binary alloys is also being investigated. The results of these subsequent experiments, together with relevant theory, will be described in later papers. The solidifying metal has been cooled in all the experiments, by a multiple air jet system designed so that the heat transfer coefficient to the cooled surface is constant and is uniformly distributed over the surface. This type of system has been chosen since only one parameter is needed to specify the heat transfer conditions and since these conditions are analogous to those met in certain continuous casting processes.' Air cooling was chosen in preference to water cooling, however, since it offers a wider range of heat transfer conditions, and since it can be investigated by analogous mass transfer techniques. The first part of this paper discusses the existing integral-profile solutions that correspond to the heat transfer conditions used in the experiments, and describes the development and use of the experimental apparatus. In subsequent sections the heat transfer and solidification results are presented, and the various theoretical predictions are compared with them, and with one another.

Jan 1, 1970

By Donald T. Hawkins, Ralph Hultgren

The lorsion effusion method has been used to measure the vapor pressure of lead over pure lead and eight Pb-Sn alloys ranging from 9.1 to 87.9 at. pct Pb in the temperature range 950° to 1125°K. The resulting ?H°y 298 = 46,630 ± 200 cal per g-atow for pure lead is in excellent agreement with previous work. Deriued ?Gph values for the alloys were smoothed and correlated with previous heat of formation data to obtain entropies for the liquid alloys. values for the tin component were calculated by Gibbs-Duhem integmtion. Surfhce depletion of these liquid alloys was found to be absent, as shown by the fact that the measured pressure remained substantially constant with time in contrast with previous measurements on iron-rich solid Fe-Mn alloys. The activities and Gibbs (free) energies of the liquid Pb-Sn system are not well known although the heats of formation have been accurately determined by K1eppa.l Vapor pressure determinations of the activity of lead by Voronin and Evseev2 disagree with those of Predel.3 Elliott and chipman4 measured activities by the electromotive -force technique in the ternary Pb-Sn-Cd system. From the resulting values of the activity of cadmium, they were able to calculate the activities of lead and tin for the binary Pb-Sn system at the compositions xsn = 0.33 and 0.67. Atarashiya, Uta, Shimoji, and Niwa5 determined the activity of tin from Hz-H2O equilibrium measurements, but their results are subject to question due to uncertainty in the final state of their samples. To resolve these differences, measurements of the activity of lead were made using a torsion-effusion apparatus. Among other advantages, this apparatus rapidly detects errors caused by surface depletion, which tends to reduce the apparent vapor pressure of the more volatile component. If the measured torques remain nearly constant with time, only bulk depletion is occurring. This contrasts with the rapid decrease in torque found in solid Fe-Mn alloys at high temperatures and low manganese contents.6 EXPERIMENTAL 99.999+ pct Pb was obtained from the American Smelting and Refining Co. and 99.999 pct Sn from Vulcan Detinning Co. Eight Pb-Sn alloys were prepared by melting together weighed amounts of the pure metals in evacuated Pyrex tubes and quenching the melts in water. Loss of weight in preparation was less than 0.02 pct in all cases. The effusion cells were made from high-purity, nonporous graphite. Graphite was chosen because of its resistance to reaction with lead and tin and because it can be accurately machined with precision orifices. Two cells were used with overall dimensions as shown in Fig. 1. The orifices of cells 1 and 2 were, respectively, 1 and 1.5 mm in diam.

Jan 1, 1968

J. T. Pullon, Rowangarth, Roundhay, Leeds, England :— In discussing Mr. Lee's paper, I wish to call attention to the fact that Mr. B. II. Thwaite (who was heard here yesterday on the subject of the application of blast-furnace gas for the production of power, of which he was undoubtedly the pioneer) read, at the Engineering Congress in Glasgow in 1901, a paper on the profitable utilization of power from blast-furnace gases,' in which he suggested the diversion and cleaning of the whole of the waste gases coming from the blast-furnace and their utilization for power-production, so as to obtain, with proper manipulation, from 4 to 6 times the efficiency of present methods. He suggested also the heating of the stoves with producer-gas of a higher and therefore more suitable calorific value, so as to maintain them in a constant state of maximum efficiency, free from dust, and to avoid the irregular working of the furnace, besides obtaining a maximum supply of air-blast, of 15 or even 20 lb. pressure, by means of internal-conibustion blast-engines driven by the cleaned waste furnace-gases, with a surplus of gas left for other uses. Since that time, in view of the necessity of having a stand-by plant, immediately available, in case of strikes or other reasons causing the banking or blowing-out of the blast-furnace, he has developed, as an addition to his other types of producer, a high blast-pressure gas-generator, producing a gas identical with, or somewhat superior to, blast-furnace gas; and in which all the ash of the fuel is turned into fluid slag, which is available for, the production of slagwool. The gas is a little richer in carbon monoxide than average blast-furnace waste gas, and has only from 1 to 3 per cent. of hydrogen. Fig. I, drawn from a photograph, shows a plant containing this generator, now in operation at Leeds. It is made in units of from 1,000 to 10,000 h.p. capacity for each vessel, and coupled,

Jan 1, 1907

By Clinton M. Young

The experiments herein described were carried on in 1908-9 by- the State Geological Survey of Kansas. Some months before taking up work on black powder the Survey had resumed work on an interrupted investigation of explosions in coalmines, a subject which is engaging the attention of numerous investigators. An unusual number of serious disasters has directed to the subject a study which discloses the disquieting fact that, in the United States, the ratio of lives lost per ton of coal mined has been 011 the increase. Methods of coal-mining have changed to some extent with the great increase of output, attained in comparatively recent years. These changes involve the working of very extensive mines, with increased difficulty of ventilation, increased accumulation of coal-dust, and a very great increase in the amount of explosive used. This last point assumes truly startling proportions when it is carefully observed. In the fields of the Middle West it is not now uncommon for a miner to use six kegs (150 lb.) of black powder in a " pay" of two weeks, while within the memory of men still active, one keg (25 Ib.) would last two men for a " pay." So great has the use of explosives become in some fields that the skilled coal-miner is hard to find, and the coal is not mined, but blasted. A preliminary study of the subject of explosions in coalmines has led to the belief that the use of large quantities of explosives, in some cases by slightly-trained men, had riot been

Jan 1, 1911

By Robert T. Walker

Robert T. Walker and Woodville J. Walker (Walker Engineering Corp., Salt Lake City)-Mr. Kinkel's article embodies, in condensed form, the results of the first detailed and complete geological survey that has ever been made of the long neglected but potentially very important West Shasta Copper-Zinc district, in Shasta County, California. In view of the difficulties of the terrain and the complexity of the geological structure, this represents a notable achievement, and it is with regret, therefore, that the writers find it necessary to differ from Mr. Kinkel's conclusions on two important points. The first has to do with the interpretation of two members of the stratigraphic column of formations in the district; for purposes of comparison, the description of these two members according to Mr. Kinkel is shown parallel to the description of these members according to the writers, see Fig. 14, Mr. Kinkel's nomenclature being used

Mar 1, 1956

By J. A. Marton, N. Brown, M. Herman

AT high temperatures a deformed polycrystalline metal shows grain-boundary displacement in preference to slip lines.' This has led to the conclusion that overall strain at high temperatures is produced chiefly by grain-boundary displacement. Detailed microscopic examinations of individual grain boundaries have shown many interesting ways by which their displacement occurs; sometimes no grain deformation was observed except possibly in the immediate neighborhood of the boundary. However, X-ray examinations show that at high temperatures subgrain formation occurs;Y he process, generally called polygonization, results from lattice bending and the subsequent climb of dislocations to form low-angle boundaries. Quantitative measures of the grain-boundary displacements show that they make a minor geometrical contribution to the overall strain; the major contribution is made by grain deformation."'" A relationship between grain-boundary displacement and grain deformation was suggested by McLean, who showed how the degree of polygonization would determine the amount of grain boundary displacement: and by Dorn, who showed that for a given creep stress, the amount of grain-boundary shear was related to the overall strain and was independent of temperature.' Although the grain-boundary displacement may make a small geometrical contribution to overall strain, it may still be the rate-controlling factor in high-temperature creep. If in general grain-boundary displacement and grain deformation are dependent quantities, then the designer of a creep-resistant metal would like to know whether it is more desirable to strengthen the matrix of the grain or to increase the strength of its boundary. The widespread interest in the relationship between temperature and grain-boundary displacement makes it desirable to test the generality of Dorn's result6 that the ratio of grain-boundary displacement to overall strain is independent of the temperature for a given creep stress. In this investigation p-brass was used because it produces sharp grain-boundary displacements above 400°C. Since B-brass undergoes an order-disorder transformation which abruptly strengthens the grain, it is an excellent metal for determining whether grain-boundary displacement or grain deformation is the rate-controlling factor in creep. The problem will be confined to the temperature range where

Jan 1, 1958

By Arthur L. Walker

In June, 1893, while I was with the Old Dominion Copper Co. at Globe, Ariz., I received an offer to take charge, as manager, of the Baltimore Electric? Refining Co. which had recently built a plant at Baltimore, Md., having a capacity of about 1200 tons of electrolytic copper per month, using the Hayden series system. This was a very large output, for in those days the plants were small and the art was in its infancy. At the beginning of 1893 there were 11 electrolytic refineries in the United States, most of them using the multiple system. The Hayden series system was used at Baltimore and Bridgeport and the Smith series system was in operation at the Electrolytic Copper Co. at Ansonia, COM., and at the Pennsylvania Salt Co. at Philadelphia. In the latter system the plates were placed in a horizontal position, but the operating difficulties were so numerous it was soon discarded. The total production of these 11 plants in 1892 was very small; I have not been able to discover reliable figures of production. There were about thirty electrolytic copper refineries in the world that year, according to Titus Ulke, and the entire production of these

Jan 1, 1932

By M. A. Westbrook, J. F. Redmond

A method is presented for obtaining porosities of consolidated formations from the drill returns. The method provides a means of determining the bulk volume of a large number of particles, such as drill cuttings, by employing a capillary diaphragm for removal of surplus surface liquid from saturated cuttings having pores of capillary size, which reduces tile amount of error present in former attempts to determine the porosity of drill cuttings. The method makes it possible to obtain a considerable amount of supplementary data on consolidated formations. Introduction Porosity is a direct measure Of the volume of the voids in a formation. It may be used for estimating the permeability of a formation provided that a correlation of these two properties has been obtained from the analysis of cores from the particular formation, and it forms a desirable aid in interpreting electric logs.1 These useful applications have emphasized the importance of developing a method for determining the porosity of the formations penetrated by a well by some means other than coring, for even in exploration wells it is neither economical nor practical to core all formations. Also, in wells where at the outset the coring program appears comprehensive, it is frequently found that, after certain layers are drilled. more complete information is required for evaluation. Porosity values, if obtainable, would be of great assistance in such cases. In soft formations it is usually possible to obtain porosities after drilling with cores taken by side-wall coring devices. In hard consolidated formations, that coring procedure is not alway practicable and other methods for determining porosities must be resorted to. A first choice is the examination of drill cuttings. if an analytical procedure is available that is both accurate and reasonably rapid. Such a procedure has been devised and is applicable to sand and limestone cuttings having pores of capillary size. Although imp,ovements can yet be made, it is believed that the new technique is sufficiently well developed to warrant description, Preparation of Sample The well samples containing the cuttings representative of the particular intervals are first washed through a No' 6 gauge screen. The cuttings remaining on the Screen are large enough to use lor the porosity measurements' From the sized sample, the cuttings to be examined are separated from the shale and Other extraneous particles. It is recommended that 10 to 15 c.c. of the selected cuttings be used for measurements, although only 4 to 5 c c. were used to make the comparative tests described later in this article. These cuttings are extracted and dried by the same methods used for preparing core samples for porosity and other measurements. The separation, which is at present being carried out by hand, is the most tedious

Jan 1, 1946

By E. W. Filer, R. P. Smith, L. S. Darken

The solubility of nitrogen gas in purified iron and low alloy steels is determined for the y region (930° to 1350°C). The diffusivtiy of nitrogen is estimated from the rate of approach to equilibrium. The investigation of aluminum-killed steels, held in nitrogen, discloses precipitation of aluminum nitride, the solubility of which is determined. ALTHOUGH several investigations of the solu-bility of nitrogen gas in y iron have been reported, all have made use of the method adopted by Sieverts in his classic work, whereby the solubility is determined by the pressure or volume change of the gas. The agreement between different investigators* is rather poor, particularly as compared to the self-consistency of results of several individual investigators. The present report represents a portion of our investigation of the equilibrium of nitrogen and nitrogenous atmospheres with iron and steels. The method adopted in this temperature region (910" to 1400°C) consists of holding the specimen in gaseous nitrogen, quenching (or cooling), and determining the nitrogen content by direct analysis (solution in acid followed by distillation and titra-tion of the ammonia).** Up to 1050°C a 20 in. vertical wire-wound (Kan-thal) furnace was used; this was wound in three sections so that by proper adjustment of relative currents, and use of a modulator1 and a commercial controller (using a chromel-alumel control couple), a zone almost 6 in. long could be maintained uniform within a few tenths of a degree. Since the temperature coefficient of the nitrogen solubility is low, the full precision was not utilized and a variation of l° to 2" was tolerated; a variation of a similar amount also occurred occasionally between the beginning and end of the experiment. At higher temperature a vertically mounted, tubular Globar furnace and control unit was used; the zone of uniformity (l° to 2"C) was here limited to about 2 in.; fluctuations with time were comparable to those in the wire-wound furnace. Reported temperatures were measured by use of a platinum-platinum-rhodium thermocouple, which was frequently com- pared with a similar standard couple which was calibrated at the gold and palladium points and also compared with one certified by the Bureau of Standards; error from this source is believed to be less than 1 "C. Nitrogen gas from a commercial cylinder was mixed with slightly over 1 pct H by use of a gas mixer described previously.' This mixture was passed over hot copper and through ascarite and phosphorus pentoxide to remove oxygen and water vapor. The purified gas contained 1.05 pct H. This procedure was adopted to prevent the formation on the specimens of oxide film, which is well known to be nearly impervious to nitrogen; its success was attested by

Jan 1, 1952

By M. A. Westbrook, J. F. Redmond

A method is presented for obtaining porosities of consolidated formations from the drill returns. The method provides a means of determining the bulk volume of a large number of particles, such as drill cuttings, by employing a capillary diaphragm for removal of surplus surface liquid from saturated cuttings having pores of capillary size, which reduces tile amount of error present in former attempts to determine the porosity of drill cuttings. The method makes it possible to obtain a considerable amount of supplementary data on consolidated formations. Introduction Porosity is a direct measure Of the volume of the voids in a formation. It may be used for estimating the permeability of a formation provided that a correlation of these two properties has been obtained from the analysis of cores from the particular formation, and it forms a desirable aid in interpreting electric logs.1 These useful applications have emphasized the importance of developing a method for determining the porosity of the formations penetrated by a well by some means other than coring, for even in exploration wells it is neither economical nor practical to core all formations. Also, in wells where at the outset the coring program appears comprehensive, it is frequently found that, after certain layers are drilled. more complete information is required for evaluation. Porosity values, if obtainable, would be of great assistance in such cases. In soft formations it is usually possible to obtain porosities after drilling with cores taken by side-wall coring devices. In hard consolidated formations, that coring procedure is not alway practicable and other methods for determining porosities must be resorted to. A first choice is the examination of drill cuttings. if an analytical procedure is available that is both accurate and reasonably rapid. Such a procedure has been devised and is applicable to sand and limestone cuttings having pores of capillary size. Although imp,ovements can yet be made, it is believed that the new technique is sufficiently well developed to warrant description, Preparation of Sample The well samples containing the cuttings representative of the particular intervals are first washed through a No' 6 gauge screen. The cuttings remaining on the Screen are large enough to use lor the porosity measurements' From the sized sample, the cuttings to be examined are separated from the shale and Other extraneous particles. It is recommended that 10 to 15 c.c. of the selected cuttings be used for measurements, although only 4 to 5 c c. were used to make the comparative tests described later in this article. These cuttings are extracted and dried by the same methods used for preparing core samples for porosity and other measurements. The separation, which is at present being carried out by hand, is the most tedious

Jan 1, 1946

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

By Irwin H. Cornell

BRIEFLY stated, the history of the St. Joseph Lead Co. is the story of how a group of men, working for ten years as officers without salaries and stockholders without dividends, developed a small mine in Missouri into what became a large and prosperous corporation. Their courage and faith in the scattered surface deposits of lead coupled with the management's engineering vision and sound financial judgment should prove an inspiration to present-day mining operators and investors. In 1717, John Law's company, known as "The Company of the West," was formed in France and letters patent were granted, for a period of 25 years by Louis XV, for exploration in the Mississippi River Valley. One of the underlying purposes of the expedition, headed by Mr. Renault and Mr. La Motte, a French metallurgist, was development of the lead mines in the area now known as Southeast Missouri.

Jan 1, 1947

By Frank H. Reed, P. W. Henline, Harold W. Jackman

A sumMary of the consumption of coal in 1945 shows that the coke industry ac-counted for 17 pct of the total coal used. No substitute for coke and the blast furnace in the reduction of iron ore has gained sufficient prominence so far to be given serious consideration. However, while the same slot-type ovens are being built and used now as were in use a few years ago, the problem of obtaining suitable coking coals, both high- and low-volatile, has forced many operators to revamp coal-blending facilities. Until the beginning of World War 11, high-temperature ooke plants were able to secure the required high-volatile and low-volatile coals from two or three seams and from three or four mines. Thus, many of our coke oven plants were able to operate with storage bins for two coals only. The vari-pnce in raw materials was not great, and uniformity of blend was a relatively simple problem. Since the beginning of World War 11, many and important changes have taken place. Demand for all coals increased greatly. Production, though kept as near maximum capacity as possible, could not meet the demands for coal generally, and particularly for the various kinds of coal which have proved to be satisfactory for specialized uses; coals were allocated as nearly as possible in the order of greatest need; storage piling was reduced to the minimum necessary to keep plants in operation; uniformity of quality could not be maintained, and with this last, uniformity of composition of blends for coking could not be maintained. Whereas before the war producers of metallurgical coke could fill their needs from three or four mines, by the end of the war it was not unusual to find shipments to a single coke oven plant coming from as many as 30 different mines, in a single month. Since many of the mines producing both high- and low-volatile coal for high-grade metallurgical coke are rapidly nearing de-pletion, the problem of seeking new sources and of blending a number of coals in each plant for the production of high-temperature coke is facing practically every producer in the United States at the present time, and is one which will probably continue for many years to come. Midwestern byproduct coke ovens in the Chicago and St. Louis areas use annually from 12 to 15 million tons of bituminous coals which are transported 500 to 700 miles from the Appalachian coal fields of Pennsylvania, West Virginia, and eastern Kentucky. Approximately two-thirds of this coal is high-volatile bituminous. The critical transportation problem confronting the nation in 1943, and the growing scarcity of the best Appalachian coking coals, prompted the Illinois Geological Survey to propose a research program in which would be studied the coking properties of blends of low-sulphur, high-volatile Illinois coal with the high- and low-volatile coals from the eastern fields. Such blends containing Illinois coal, if substituted for the all-eastern blends normally coked,

Jan 1, 1949

By J. E. Hilliard

Isobaric sections of the eutectoid region of the iron-carbon phase diagram have been exgerimentally determined at 35, 50, and 65 kb. The phase boundaries were located by metallographic analysis of specimens quenched after equilibriatwn at known temperatures and pressures. With increasing pres -sure a pronounced decrease in the solubility of FesC in austenite was observed together with a depression of the eutectoid temperature. These two effects resulted in a shift of the eutectoid composition toward a lower carbon content; at 65 kb the eutectoid was at less than 0.2 wt pct C. These results are in qualitative agreement with thermodynamic calculations. It has also been shown by calculations that Fe3C in contact with saturated austenite will be stable with respect to both graphite and diamond formation at all pressures above -3.5 kb. 1 HE investigation described in this article was part of a more general study of the effect of high pressure on transformations in Fe-C alloys. Thermodynamic calculations and exploratory runs made in 1959 at the start of the program indicated an appreciable change with pressure in the phase equilibria of Fe-C alloys. However, the calculations were not considered reliable enought to provide the quantitative information required for the interpretation of the effect of pressure on the kinetics of transformations. An experimental investigation was therefore made to determine a series of isobaric sections of the eutectoid region of the phase diagram at pressures up to 65 kb. EXPERIMENTAL PROCEDURE Materials. Seven alloys with analyzed carbon contents of 0.10, 0.20, 0.38, 0.60, 0.77, 0.93, and 1.20 wt pct C were prepared from Ferrovac" iron and high-purity graphite induction melted in magnesia crucibles under argon. The ingots were hot worked and swaged down to 0.19-in.-diam rod which was then centerless ground to a final diameter of 0.125 in. Samples for chemical and spectrographic analyses were taken from each end of the rods. The prin- cipal impurities were found to be Ni, Al, Co, and Si which were present in amounts up to 0.03, 0.02, 0.01, and 0.01 wt pct, respectively. Specimens were prepared by slicing the ground rods into pills 0.06-in. thick which were silver plated to reduce decarburization during the equilibration. Silver was chosen for this purpose because of its very low solubility for carbon and its mutual immisicibility with iron. High-Pressure Apparatus. The high-pressure runs were carried out in the "Belt" apparatus.' As shown in Fig. 1, this consisted of a cylindrical cell compressed between two Carboloy punches loaded by a uniaxle press. Radial support to the cell was given by the "belt" which was a Carboloy die heavily prestressed by a series of steel binding rings. Laminated gaskets of lava and metal separated the punches from the inner surface of the "belt". A cross-section of the high-pressure cell is shown in Fig. 2. Two specimen pills were located inside a resistance heater of 0.20-in.-diam Nichrome tubing. The ends of the tube were sealed with alumina and lava pills tamped in place after the

Jan 1, 1963

By John C. Calhoun, F. W. Gooch, J. P. Everett

The results of two sets of displacement experiments are reported. In the first set of experiments various solutions of sugar in water were displaced by other solutions of sugar in water. In the second set oils were displaced by water. Each set of experiments was performed on a linear system made of cemented silica sand grains. These displacement tests were made to evaluate the behavior when the ratio of fluid viscosities between the displacing and displaced phases was varied. A further consequence of the test results is a comparison between displacement behavior when the displaced and displacing phases are miscible as with sugar solutions and when they are immiscible as with oil and water. INTRODUCTION Buckley and Leverett1 have presented a theory for the displacement of oil by gas or water based upon the relative permeability concept. This theory presents the displacement of oil as occurring in two phases, an initial or primary phase preceding the breakthrough of the displacing phase and a subordinate or secondary phase during which both oil and the displacing phase flow simultaneously through the same porous section. These authors gave the results of calculations to show that the percentage of oil displaced during the primary phase by water drive would be dependent upon the ratio of the viscosity of the oil to that of the water. No experimental evidence was reported by these authors to substantiate their theory. Qualitatively, however, it has been found to be in agreement with many observed field results. Laboratory investigators have been in general agreement in reporting for air or gas drive2,3 a small primary phase of production and a large secondary phase. Reported investigations on water drive3,4,5 have shown instances where both primary

Jan 1, 1950

By T. N. McVay, E. E. Creitz

Rather large amounts of titanium minerals and some zircon and monazite are being recovered from dune sands about I. miles west of Jacksonville Beach, Fla. The Mining Branch of the Bureau of Mines, Southern Experiment station, has been interested in developing additional large deposits of similar sands in other areas of Florida. The results of a field study have been published1 concerning the sands occurring on Trail Ridge which runs north and south about 30 miles southwest of Jacksonville. This investigation was undertaken in order to identify the opaque titanium minerals occurring in Trail Ridge and because of the economic importance of Florida titanium minerals. Nature of the Problem The minerals present in the heavy fractions (sp gr > 2.94) of the sands are principally opaque minerals; staurolite, zircon, sillimanite, tourmaline, kyanite, rutile, a small amount of corundum, traces of the zinc spinel gahnite and garnet. Epidote, monazite, hornblende and ti-tanite are present in other dune sands but these minerals were not noted in the samples collected on Trail Ridge. All of the minerals except those which are opaque can be readily identified by the usual petrographic methods. However, Opaque minerals cannot be examined satisfactorily by transmitted light. Polished sections of the opaque-mineral grains were examined but these sections did not furnish useful information. Consequently, it was necessary to use means other than the usual petrographic methods to identify them. Previous Investigations of Heavy Minerals in Florida Sands Martens2 has described the heavy minerals in the Florida beach sands and has classified the opaque minerals as ilmenite with minor amounts of leucoxene. Miller3 studied a number of sands collected by Ross and Mertie in Florida. He states that the material from the Florida beach and dune sands that commonly has been called ilmenite has essentially the chemical composition of the material that has been called arizonite.4 The x ray diffraction patterns of several samples indicated that the supposed ilmenite is essentially amorphous, with only weak lines corresponding to ilmenite, and hence the material is unlike the type of arizonite from Arizona. Opaque Titanium Minerals Rutile is essentially titanium dioxide. However, as pointed out by Dana,5 important amounts of Fe+2 and Fe+3 as well as Cb and Ta are reported in some analyses.

Jan 1, 1949