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By F. V. Shallcross

Physical properties of thin films of CdS and CdSe formed by vacuum deposition onto glass sibstrates have been studied as a function of deposition and processing conditions. The crystallinity and surface features of CdS films were examined using electron microscopy and electron and X-ray diffraction techniques. The films were poly crystalline; the preferred orientation and crystallite size increased with film thickness, substrate temperature, and deposition time. The CdS films consisted primarily of hexagonal-phase material, in contrast to similarly prepared CdSe films which have previously been observed to contain mixtures of cubic and hexagonal phases. As-deposited CdS films showed no major dependence of Hall mobility on crystallite size or degree of preferred orientation. Hall mobility and carrier concentration in CdS and CdSe .films were measured at various temperatures; both parameters increased with temperature and yielded activation energies which depended on fabrication conditions. Surface-desorption phenomena and overcoating of the semiconductor with SiO affected the observed electrical properties significantly. THIN films of cadmium sulfide1,2 and cadmium sele-nide3,4 have been employed by various workers as semiconductors in the insulated-gate thin-film field-effect transistor, known as the TFT. These devices are most commonly made by vacuum deposition of all materials onto an amorphous substrate such as glass. A knowledge of the microstructure and electrical properties of semiconductor layers used in the thin-film transistor is essential in order to form a realistic model for the device and to improve its performance, reproducibility, and reliability. This paper will describe studies of the physical properties of vacuum-deposited CdS and CdSe films prepared under various conditions. Structural characteristics examined in- cluded phases present, crystallite size, nature of preferred orientation of crystallites, surface roughness, and structural homogeneity throughout the film thickness. Electrical properties measured were Hall mobility and conductivity and their dependence on temperature and ambient. Thin-film properties are affected by many fabrication parameters including purity and physical form of evaporant, deposition rate, film thickness, design and temperature of the evaporation crucible, geometry of the deposition chamber, nature of the residual atmosphere, composition and temperature of the substrate, and details of postdeposition processing. PREPARATION OF FILMS In this work the semiconductor films were deposited in a conventional oil-diffusion-pumped system with pressures in the 10-8 torr range. The CdS evaporant was obtained from the Eagle-Picher Co. as a high-purity coarse-grained crystalline powder; the CdSe was a high-purity sintered powder supplied by the Harshaw Chemical Co. The evaporation crucible was a resistance-heated molybdenum-wire basket coated with aluminum oxide and filled with a quartz wool plug at the top. The source to substrate distance was usually 10 cm. This region was enclosed by a Pyrex inner cylinder. The substrate was heated with an overlying Pyrex plate coated with tin oxide. The substrate temperature was controlled using a thermocouple attached to the lower side of the heater. This thermocouple was calibrated against another thermocouple attached to a dummy substrate and by observation of melting points of various metal films deposited in the system. The substrates were polished borosilicate glass plates and conventional glass microscope slides. Substrate preparation included cleaning with an ultrasonically agitated detergent bath followed by isopropanol-vapor de-greasing. Film thickness was measured interferomet-rically during and after deposition. STRUCTURE OF CdS FILMS Structural studies were performed on CdS films using electron diffraction, electron microscopy, and

Jan 1, 1967

By Strathmore R. B. Cooke

That calcium will activate quartz for flotation with anionic collectors such as soaps has been known for a number of years,1 2 3 and the method has been applied to the concentration of various iron ore 4 5 6 as well as to other materials. Clemmer gives the permissible pH range for the activation of quartz by calcium as between 9.5 and 12.5 with an optimum value of 11.0, and Hertzog7 has determined the calcium abstraction of iron ores and of Ottawa sand, but otherwise little quantitative data are available. The purpose of the present investigation was to determine those conditions under which dilute solutions of calcium chloride will activate quartz for anionic flotation and to determine the amount of calcium ion adsorbed by quartz. Those variables, the influence of which was primary, such as calcium, sodium, and hydrogen ion concentrations, were studied. Other factors which influenced the results are discussed in the description of the experiments. Three different experimental methods were used to determine the activation of the quartz. The first method was to treat a sample of ground, deslimed quartz with solutions of calcium chloride and sodium hydroxide, and to determine the calcium adsorbed by chemical analysis of the solution. Ad- vantages are that a direct value for the

Jan 1, 1949

By Roy E. Dickerson

CUBA differs considerably from the other Greater Antilles in many geologic fundamentals. Cuba is geosynclinals; whereas Jamaica, Hispaniola. (Haiti), and Puerto Rico are geoanticlinal. (Scliuchert, Chas., Historical Geology of the Antillian. Caribbean Region, p. 13, 1935.) Rocks of lowermost Cretaceous age exist in large volume in Cuba, where- as they are generally absent in the other islands. Since many of the surface indications of petroleum are intimately associated with lowermost Cretaceous rocks, the Vinales limestone,, this difference is most important. The Vinales limestone in many places in Pillar del Rio and Santa Clara provinces reeks with light tars when broken with a hammer. The late David White and his associates on the U. S: Geological Survey studied

Jan 1, 1937

By J. F. Lewis

Much has been written on this great engineering work, principally from the civil engineer's stand-point. In presenting the subject to the Institute, it seems necessary to include something of geology as well as engineering. In this case, it is particularly the glacial and post-glacial periods with which we are concerned; for it has been clearly proved that the canal recently excavated has not for the first time opened the Des Plaines valley for drainage away from Lake Michigan, and that this valley, as well as the site of this city, is very closely connected with the processes and effects of the ice period. We have simply renewed a channel and a drainage direction which formerly existed. As the days of deep water-ways for commercial purposes are fast approaching, engineers may find the consideration of ancient topography and geologic changes highly useful. For what I may say on this subject I am greatly indebted to Mr. Ossian Guthrie, who has made an earnest study of glacial geology and labored especially to decipher the records of its history in this region. * Chicago is situated in the track of one of four great glacial ice-streams that swept down from the North: one moving due South from Marquette and entering the Illinois valley at Ottawa; one through the Lake Michigan valley, entering the Illinois valley near Lemont; one from Saginaw Bay diagonally across the States of Michigan and Iadiana, entering through

Jan 1, 1898

By N. J. Grant, E. Gregory

The creep rupture properties of wrought aluminum powder products made from five grades of sintered aluminum powder were investigated at temperatures from 400° to 900°F for rupture times up to 1000 hr. The effect of stress concentrations on materials of this type was investigated by means of notched creep rupture tests. A tentative correlation was obtained between the creep rupture properties and the structure as revealed by electron micrographs. SEVERAL papers have been published recently concerning the production and properties of wrought aluminum powder products and their possible high temperature applications. Most of the published work in this field has come from abroad, notably Switzerland, and articles by Irmann and his colleagues were summarized in English recently.'.' Most of the papers published by Dr. Irmann are principally concerned with the retention of properties (by a product which is produced from extremely fine flake powder and is subsequently hot extruded) after heating to high temperature for prolonged times. The powder may be in atomized or flake form, and during hot working the applied pressure is reported to plastically deform the aluminum powder, thus breaking the oxide skin and welding the particles together. Irmann attributes the remarkable properties to the dispersion of oxide inclusions. Specifically, the product described by Irmann is one labeled SAP (Sintered Aluminum Powder) in which the initial flake powder is so fine that at least 50 pct of the flakes have one dimension of 2 microns or less. The composition of the starting aluminum shows in percent, Fe, 0.18; Si, 0.19; Zn, 0.06; Ti, 0.03; Cu, Mn, Mg, all nil; balance Al, approximately 99.5 pct. Aluminum is not the only material that has been found to have increased resistance to deformation at elevated temperatures when produced by powder metallurgy. It has been reported by Middleton, Pf eil, and Rhodes- hat platinum has a higher recrys-tallization temperature when produced by powder metallurgy and exhibits peculiar properties, many of which are similar to those of the aluminum powder products. Difficulties were encountered in explaining the reason for the strengthening in the case of platinum since the existence of the oxide is doubtful. The authors attributed the special properties to "a small amount of suitably dispersed porosity." This theory was supported by von -~eer-leder4 in the discussion to the paper, and the similarity between this method of hardening and that suggested by Rohner in his theory of age hardening was pointed out. R. de Fleury5 attempted to explain some of the properties in terms of the modulus of elasticity and elastic limit of alumina and aluminum while von Zeerleder examined the relationship between the yield strength and the reciprocal of the powder particle size. Boenisch and WiderholtQ dealt mainly with the corrosion resistance of the powder aluminum material and compared it with other aluminum alloys. The diffusion rates of other metals in SAP and pure aluminum have been compared by Seith and Lop-mann.' They showed that the alloying metals diffuse particularly quickly in SAP possibly due to the very fine grain size. The properties of the Alcoa products were given by Lyle.' The creep rupture properties of SAP and two of the Alcoa experimental powder products were compared by Gregory and Grant hnd it was shown that these products are vastly stronger at 900°F than are the best cast and wrought alloys at 600°F. Since the publication of these data, the authors have investigated two further aluminum powder products and it is the object of this paper to show how the high temperature creep rupture properties of the five materials vary with oxide content and with the structure as revealed by electron microscopy. Materials One of the five products, SAP, a sintered aluminum product, was supplied by the Societe Anonyme pourl Industrie de l,Aluminium, Neuhausen a/RHF, Switzerland, through Dr. R. Irmann, while the others, M276, M257, M293, and M255 were supplied by the Aluminum Company of America as experimental powder metallurgical products. M255- and M293 were made from coarse and fine atomized powders, respectively. The other materials were made from flake powders with significant differences in oxide content, the details of the type of powders used in the manufacture of these materials

Jan 1, 1955

By Edward P. Barrett

DURING the past few years numerous references have been made in the technical press and Bureau of Mines Bulletin 270 to sponge iron' and so-called "direct metal" processes. The idea has been prevalent that sponge iron and "direct metals" are cheap commodities. In many instances it has been proposed that these processes be used to treat low-grade ores, utilizing low-grade coals as reducing agents. It is questionable whether or not high-grade sponge iron can be made from low-grade materials. Particles contain¬ing iron oxide and gangue become, upon almost complete deoxidation, particles containing metallic' iron and gangue. The possibility of mechanically separating the metallic iron from the gangue in these particles depends . on the physical characteristics of the particular ore under treatment. Some ores, in which the minerals constituting the gangue break free from the iron oxide upon crushing, may be concentrated magnetically after the iron oxides have been reduced to metal. The finely disseminated ores are least amenable to concentration. In general, high-grade sponge iron can only be made from high-grade raw materials. Sponge iron containing small amounts of sulfur can only be made from raw materials containing small amounts of sulfur or by

Jan 1, 1930

By R. Schuhmann Jr., P. J. Ensio

As a first step in a study of the physical chemistry of copper-smelting slags, experimental measurements were made of the oxygen pressure of simple iron-silicate slags in equilibrium with solid iron. The experiments consisted in bubbling CO2-CO mixtures through the slags in iron crucibles and in finding the equilibrium ratios of CO2 to CO. From the data, activities and partial molal heats of solution FeO and SiO2 in the slags were calculated. THE ternary system FeO-Fe,O,-SiO, is the simplest system which can represent adequately the important chemical properties of the slags formed in matte smelting and converting. Accordingly, the experimental study of slags in this system was started as the first step in a general research program on the thermodynamics of copper smelting. A recent paper by one of the authors' outlines this general research program and shows in some detail how information on thermodynamic properties of iron-silicate slags, especially information on oxygen activities, is essential to a full understanding of the chemistry of copper smelting. The FeO-Fe,O,-SiO, system also is the basis of slags produced in other processes, such as acid steelmak-ing processes, and is important in relation to the behavior of silicious refractories. In addition, data on the physicochemical properties of iron-silicate slags should contribute to a general understanding of the nature of slags, since at present such data for all kinds of slags are relatively meager. The principal quantitative information already available on iron-silicate slags consists in Bowen and Schairer's constitution diagram for slags in equilibrium with metallic iron,' Darken and Gurry's complete and precise thermodynamic study of the Fe-0 system,",' and Darken's study of the phase equilibria in the Fe-Si-o system. From the results of this previous work, it was clear that a complete thermodynamic study of ternary iron-silicate melts was a major undertaking which would have to be broken down into parts, including the working out of the ternary equilibrium diagram as well as extensive activity measurements on slags. The experimental measurement of oxygen activity, using CO-CO, and other gas mixtures as yardsticks of oxygen activity, was the basis of Darken and Gurry's study of the Fe-0 system. From the experimental measurements of oxygen activities over a large range of temperatures and compositions, they were able to calculate the activities of other species such as Fe, FeO, Fe,O,, etc., and also the other important thermodynamic properties in the Fe-0 system. At the start of the present investigation, it appeared that the same approach would be fruitful for the study of iron-silicate melts. Also, the experimental measurement of oxygen activities seemed particularly attractive because oxygen activity itself is a quantitative measure of oxidizing or reducing power, which is an important variable in copper-smelting slags. The slag compositions in equilibrium with yFe appeared most suitable for the first investigation of this kind, for the following reasons: 1—Good constitution data2 were available. 2—An iron crucible could be used, thus affording a simple solution to the refractory problem without introducing contarnination. 3—With Fe activity fixed, at unity with respect to a standard state of solid Fe, measurements of 0 activity could be followed by simple calculations of activities of FeO and other Fe-0 complexes and of SiO,. 4—This starting point afforded several possibilities for cross-checking with previous work,

Jan 1, 1952

By Robert Adams

Secondary or scrap materials appear at all stages in the industrial process and in a bewildering variety of forms, grades, and values. It is useful to begin analyzing them by dividing the broad concept of "Secondary Supply" into three parts First, the concept must encompass the stock, or pool, of secondary materials. In the process of satisfying his wants, man produces desired products from the materials and natural resources found around him. As long as the rate of production is greater than the rate of obsolescence of a given product, the total stock or pool of materials embodied in that product will increase in size This stock concept relating to secondary materials is directly analogous to the "resource" concept used for primary raw materials in the preceding chapter, and includes all materials embodied in existing products (Obviously, this excludes those materials which are destroyed in the consumption process, viz , fuel oil burned to provide heat.) Consumption of a primary material in a productive process tends to reduce the resource base of that primary material In direct contrast, however, the production or use of products increases the resource base of the secondary material. Thus, we find that a country which has no resource of a primary material can, by importing products that contain the material, build up a large enough stock to provide a basis for secondary recovery. The estimated growth of the pool of copper in use in the United States through 1967 is shown in Table 5.B.1.a The estimate of 39 3 million tons at the end of 1967 includes only technologically recoverable copper and is, therefore, somewhat less than the stock concept described previously, which does not distinguish between recoverable and unrecoverable material. Nevertheless, Table 5 B.1 does give an idea of how a nation's secondary resource of a material can grow over the years. A second aspect of the concept of secondary supply is the generation of secondary materials. This includes materials generated as scrap in production as well as the movement of a material out of the stock of existing products via wear, damage, or obsolescence The quantity of materials generated is usually either nearly or completely independent of the technologic capabilities and economic forces which prevail in the secondary recovery market.b The justifications for and the qualifications to this statement are considered later. The final aspect of the concept of secondary supply consists in the secondary recovery process It is at this point that the technologic and economic forces of the secondary recovery market become the controlling fac-

Jan 1, 1976

By John Hall

SOME months ago one of the authors was asked to write a paper on the heat treatment of steel castings that would be more comprehensive than other matter lie had published; this is an attempt to present in condensed form the results of experimental work and actual practice carried out for the most part in 1907, 1908; and 1909. It is not a laboratory research and the work done was carried out for the express purpose of putting in practice the processes discovered as fast as possible. Most of the tests are the result of commercial practice and not of bars annealed in our laboratory; most of the micrographs were made for our own records and not for publication. Certain of the micrographs, therefore, are not as clear as we may wish but they were good enough for our purpose at the time they were made. The tests and micrographs are selected from several thousands in our files. All of these micrographs are magnified 60 diameters. These experiments were conducted almost entirely on steel made in a 3-ton bottom-blown converter, and most of the steel illustrated analyzes about 0.05 in phosphorus and sulfur. Unfortunately, a certain number of specimens are shown of which we do not have the complete analysis, but in most cases in which the phosphorus and sulfur vary much from the figure just given that fact is noted. For purposes of comparison, we have included a certain number of micrographs and tests of steel made in the electric furnace, some of which were from specimens made in other shops and some in our own shop, and some tests of acid open-hearth and tropenas steel.

Jan 9, 1919

By AIME AIME

FREE competition, long the controlling ideal of domestic trade within the United States, has had the fundamental geographical advantage of functioning in the world's largest area of unrestricted commerce. Goods moved back and forth across state lines, unimpeded by customs, and industrial operations have developed rapidly to meet the expanding needs of a pioneer country richly endowed with natural resources. Fifty years ago, antitrust laws were adopted to protect the competitive private enterprise principle. It became illegal for one person to combine with another to restrain trade or commerce among the several states or with foreign nations. The original legislative measures defining this philosophy were the Sherman Act of 1890 and the Clay- ton Act passed in 1914. The development of Europe and other parts of the world was influenced by different conditions which led to a different theory of trade. Here were many small nations, with limited natural resources and a thin market, and they attempted to protect their national economy by tariff walls. International business arrangements for the purpose of diminishing the ups and downs of the more competitive system --crux of the modern cartel operations-seemed a logical device to stabilize production and guard the interests of both workers and consumers. European governments as well as European industrial interests became convinced that if com- petition could be held in bounds the danger of business depressions and un- employment could be reduced.

Jan 1, 1944

By W. H. Herrnstein, J. B. Clark, E. C. Utley, A. J. McEvily

The ratio of the endurance limit (10' cycles) to tensile strength of age-hardened aluminum alloys is approximately 0.3, whereas the ratio for annealed alloys is about 0.5. The lower value for the age-hardened alloys has been associated with the instability of coherent precipitate during cyclic loading, but it has not been definitely established whether this instability is due to overaging or reversion during cyclic loading. The results of the present investigatzon support the reversion viewpoint. In this work specimem of 2024-T4 aluminum alloy were aged for 16 hr at 150°C after cycling for 10 pct of the life at 25.000 psi. These specimens were then tested to failure and exhibzted a marked increase in fatigue life. It is proposed that during the early stages of fatigue in this alloy dislocations cut through the coherent precipitate and bring about the reversion of the precipitate. Subsequent aging at 150ºC induces reprecipitation in the precipitate-free zones so that the weakened regions are strengthened and the fatigue life is extended. It Is recognized that the fatigue strengths of precipitation hardened aluminum alloys are unusually low relative to their tensile strength.'-= This feature is illustrated in Fig. 1 where it can be seen that age-hardened alloys have lower fatigue ratios (the ratio of the fatigue strength to the tensile strength) than those in the annealed or cold worked state. Further, as shown in Fig. 2, the more an alloy is dependent upon precipitation hardening for its total strength, the lower is the ratio of the fatigue strength to the tensile strength. This state of affairs has been associated with an instability of the metastable metallurgical structure of precipitation hardened aluminum alloys during cyclic loading. Evidence2 in support of this view is that the fatigue ratio increases in these alloys as the test temperature is lowered, thereby indicating that thermo-mechanical instability, rather than some other factor such as a non-uniform distribution of precipitate, is the factor responsible for the low fatigue ratio at room temperature. Two mutually exclusive proposals have been ad- vanced to account for this instability. Hanstock has proposed that overaging takes place during cyclic loading, and in support of this view, Broom et a1.2 have indicated that an overaging process might be promoted by the large numbers of vacancies which are created during cyclic loading. The creation of vacancies by radiation4 has been shown to lead to rapid overaging. Hanstockl obtained visual evidence of overaging in an aluminum alloy after cyclic loading, but in this instance it has been pointed ou? that because of the high frequency used (60,000 cpm) the observed effect may have been due to normal high temperature precipitation around energy dissipating cracks. Efforts to discern visual evidence of overaging in this alloy at lower test frequencies were not successful.3 The alternative postulate3 is that reversion takes place during cyclic loading and leads to localized soft spots at which fatigue cracks are readily initiated. Evidence for this process has recently been provided by Polmear and Bainbridge5 who demonstrated metallographically that regions depleted of precipitate were created during cyclic loading of an aluminum alloy. Inasmuch as precipitate particles bordering the depleted region had not grown in size, it was concluded that the solute atoms which had constituted the missing particles had gone back into solution. No mechanism for the reversion process was presented. The present study was undertaken to investigate further the conditions leading to instability during cyclic loading, and to determine whether reversion or overaging had taken place as a result of cyclic loading. BACKGROUND AND TEST PROCEDURE In order to differentiate between the processes of reversion and overaging, rest periods at an elevated temperature, which ordinarily would insure additional precipitation, were used in this investigation. It was expected that after a period of cyclic loading an elevated temperature rest period would result in a decrease in the remaining life of the specimen if overaging were occurring during cyclic loading, whereas in the case of reversion, reprecipitation would occur and the fatigue life would be extended. Such an expectation is based on the assumption that the crack-nucleation phase is a significant portion of the total fatigue life, and that such a treatment is of influence in the crack-nucleation stage and is relatively unimportant thereafter.

Jan 1, 1963

By A. B. Hersberger, R. S. Dean

Although it is obvious that in any flotation process we must have a froth, in recent years the development of collecting reagents has caused the possibilities of better frothing agents to be overlooked. Some investigators have even gone so far as to say that the number of satisfactory frothing agents was sufficient. A little consideration will show, however, that the reagents available in the past were far from ideal frothers. The properties of an ideal frother for flotation work may be set down as follows: 1. It must form in low concentrations a copious but not too persistent froth. 2. It must be insensitive to hydrogen-ion concentration of the pulp; that is, it must froth equally well in an acid or alkaline medium. 3. It must be insensitive to salts, even in high concentration. 4. It must be absolutely noncollecting to both sulfides and nonsulfides. 5. Its frothing properties must not be affected by collecting reagents, including soap, the most generally used nonsulfide collector. 6. It must readily emulsify and disperse any insoluble collecting agent that is likely to be used. Clearly the existing frothers do not qualify. Pine oil, for example, is an acceptable frother for many purposes but if used in soap flotation a delicate balance between pine oil and soap must be struck because, as pointed out by Coghill1, these two reagents are incompatible in certain concentrations. The objections to soap itself as a frother are obvious, and the cresols and their substitution products all have some collecting power and very little emulsifying power. The mechanism of frothing in flotation was early explained on the basis of the Harkins-Langmuir theory of oriented molecules.2 These investigators showed that if an organic compound having an unsym-metrical molecule (in which one end of the molecule contained water-

Jan 1, 1939

By R. S. Dean, A. B. Hersberger

Although it is obvious that in any flotation process we must have a froth, in recent years the development of collecting reagents has caused the possibilities of better frothing agents to be overlooked. Some investigators have even gone so far as to say that the number of satisfactory frothing agents was sufficient. A little consideration will show, however, that the reagents available in the past were far from ideal frothers. The properties of an ideal frother for flotation work may be set down as follows: 1. It must form in low concentrations a copious but not too persistent froth. 2. It must be insensitive to hydrogen-ion concentration of the pulp; that is, it must froth equally well in an acid or alkaline medium. 3. It must be insensitive to salts, even in high concentration. 4. It must be absolutely noncollecting to both sulfides and nonsulfides. 5. Its frothing properties must not be affected by collecting reagents, including soap, the most generally used nonsulfide collector. 6. It must readily emulsify and disperse any insoluble collecting agent that is likely to be used. Clearly the existing frothers do not qualify. Pine oil, for example, is an acceptable frother for many purposes but if used in soap flotation a delicate balance between pine oil and soap must be struck because, as pointed out by Coghill1, these two reagents are incompatible in certain concentrations. The objections to soap itself as a frother are obvious, and the cresols and their substitution products all have some collecting power and very little emulsifying power. The mechanism of frothing in flotation was early explained on the basis of the Harkins-Langmuir theory of oriented molecules.2 These investigators showed that if an organic compound having an unsym-metrical molecule (in which one end of the molecule contained water-

Jan 1, 1939

By J. H. Yang, K. E. Gray

Results of single-blow bit-tooth impact tests on saturated rocks under elevated confining pressures and zero pore pressure were reported in a previous publication.1 This paper presents an extension of the earlier work to include a study of crater formation during tooth impact on both gas- and liquid-saturated Berea and Bandera sandstones at elevated confining and pore pressures. The basic data obtained were force-time, displacement-time, velocity-time and force-displacement curves during crater formation. Crater volume was also measured and the mode of crater formation determined. Bit tooth geometry, depth of penetration and velocity of impact were held constant. Results indicate that, with pore fluid present in the rock, failure trends from brittle to ductile as pore pressure is increased at constant confining pressure (pore pressure and borehole pressure were equal) For a given rock type, the mode of crater formation was dependent not only upon the nominal effective stress, but also upon the fluid which saturated the rock pore space. When confining pressure and pore pressure were equal (zero nominal effective stress), bit-tooth impact resulted in brittle failure for nitrogen-saturated Berea, and brittle to transitional failure for nitrogen-saturated Bandera; when saturated with liquid both rocks failed in a ductile manner at zero nominal effective stress. INTRODUCTION Dynamic wedge penetration tests have been conducted by investigators in several fields, but the failure mechanism of rock under dynamic stresses is not understood completely. The complex action of drilling bits, even considering the action of a single tooth, may be considered as a combination of drag bit and rolling cutter action. Thus, as a first step in understanding rock breakage in oil well drilling, single chisel impact and rock planing are of fundamental importance. For example, Gray 2 and Crisp3 studied drag bit cutting action at brittle stress states. Simon4 and Hartman5 studied the reaction of rocks to vertical impact by means of drop tests. The depth of penetration, crater volume and force-vs-time curves during crater formation were observed. The significance of indexing single-bit impacts has been noted.4,6-8 Gamer et al,9 reported impact tests on impermeable Leuders limestone at atmospheric and elevated confining pressures. In all cases the tests were accomplished on dry rock and pore pressure was considered to be zero. The importance of both confining pressure and pore pressure on the failure characteristics of rock was described. 10-12 It was found that the yield strength and ductility of porous rock depend on the state of stress under which the sample is tested. The importance of pore pressure on drilling rate in microbit experiments was noted by Cumingham and Eenink. l3 Robinson 12 also pointed out that in drilling the most important parameter in rock failure is the effective stress, where effective suess is defined as confining pressure pc minus pore pressure pp. The effect of pore pressure and confining pressure on rock strength was also noted by Serdengecti and Boozer 14 in strain rate tests, and by Gardner, Wyllie and Droschackl5 in elastic wave studies. Until recently all reported wedge impact studies under simulated wellbore stress states have been conducted on dry rock. Maurer 16 reported impact tests on samples saturated with deaerated water. Borehole and formation fluid pressures were equal in these tests except when mud was used in the borehole. With mud in the borehole and a high borehole-to-formation fluid pressure differential. Maurer observed "pseudoplastic" crater formation. Podio and Grayl reported impact tests on Berea and Bandera sandstone saturated with pore fluids having wide ranges in viscosities. In Podio and Gray's tests, confining pressure was elevated, but pore pressure and borehole pressure were held fixed at atmospheric pressure. The presence of

By AIME AIME

COAL occupied a large place in the technical sessions of the Institute at its annual meeting for in addition to three sessions specifically de- voted to coal the two sessions on mine ventilation and the two on ground movement and subsidence, which are reported under their own headings, were primarily concerned with coal. The first session on coal was a joint one with the Iron and Steel Division, on Wednesday afternoon, with F. H. Crockard and J. R. Campbell presiding as joint chairmen and the latter actually officiating. The principal topic of discussion was G. S. Scott's paper "Evaluation of Coal for the Making of Blast- Furnace Coke," which has been published as T. P. 159. The author made a brief statement of its con- tents to start the discussion and the chairman, after briefly reviewing it himself, called on C. A. Meissner to start the discussion. He briefly reviewed the economic factors in the use of coal for coke-making, saying that not only .does the removal of 1 per cent of ash from the coal reduce the cost of pig iron 12 or 13c. per ton, but it also permits coke of satisfactory structures to be made from a coal which otherwise could not be used. He stressed the importance of uniformity in blast-furnace fuel and discussed the benefit of mixing different coals as raw material for the coke oven and cited experience with Illinois coals.

Jan 1, 1929

By Albert A. Smith

The creep properties of metals have assumed increasing importance in recent years and many investigations have been made on various phases of the problem. In the past year the annual lectures of the Institute of Metals Division1 and the Iron and Steel Division2 were concerned with this subject, and are excellent reviews. For many years the creep properties of lead and lead alloys have been investigated at the Central Research Laboratories of the American Smelting and Refining Co., and it is hoped that the present paper will contribute knowledge of some of the factors that influence creep. Lead, being a metal that recrys-tallizes readily at room temperature, is an excellent material upon which to investigate creep phenomena because of the simplicity of the apparatus needed, and it might be expected that results would apply to some extent to elevated-temperature tests of other metals. Material The creep tests of this investigation were all made on high-purity lead (99.9998+ Pb) in which the only impurity that could be detected by spectrographic and chemical means was approximately 0.0001 per cent Fe. Flat strips, 0.750 in. wide by 0. 100 in. thick, were prepared by extruding 2-in. dia. cast billets at a temperature of 250°C. This gave a material of 2 to 3 mm. average grain size with a tensile strength of j.400 lb. per sq. in. when tested at a straining rate of 5 per cent per minute. With this extremely soft material, great care was necessary in handling the specimens, to avoid distortion and subsequent recrystallization. The creep tests at 30°C. were conducted in a constant-temperature room, specially built for the purpose in the basement of an office building in which there was no moving machinery, and no vibration was detectable under the most severe conditions of shock in the adjacent surroundings. The room was well insulated and heated electrically, control being by means of a de Khotinsky regulator operating a relay. Maximum temperature variation over a period of several years has been ± 1/2°C. Specimens of the extruded strip, 16 in. long, were used for test purposes with no reduced gauge section, thus eliminating any distortion due to machining. The method of clamping and supporting the specimens is shown diagrammatically in Fig. 1. The gauge marker for the measurement of extension consisted of an aluminum strip, 0.050 in. thick by 0.75 in. wide, one end of which was ground and sanded to a precise knife-edge and fastened to the specimen by suitable pins. After the strip was fastened in place a fine scratch was inscribed just below the knife-edge by means of a sharp teasing needle. Just below this gauge scratch a short vertical mark was made so that the same point could be located and read each time. Several hundred specimens have been prepared by this method, and it was found that with experi-

Jan 1, 1941

By Albert A. Smith

The creep properties of metals have assumed increasing importance in recent years and many investigations have been made on various phases of the problem. In the past year the annual lectures of the Institute of Metals Division1 and the Iron and Steel Division2 were concerned with this subject, and are excellent reviews. For many years the creep properties of lead and lead alloys have been investigated at the Central Research Laboratories of the American Smelting and Refining Co., and it is hoped that the present paper will contribute knowledge of some of the factors that influence creep. Lead, being a metal that recrys-tallizes readily at room temperature, is an excellent material upon which to investigate creep phenomena because of the simplicity of the apparatus needed, and it might be expected that results would apply to some extent to elevated-temperature tests of other metals. Material The creep tests of this investigation were all made on high-purity lead (99.9998+ Pb) in which the only impurity that could be detected by spectrographic and chemical means was approximately 0.0001 per cent Fe. Flat strips, 0.750 in. wide by 0. 100 in. thick, were prepared by extruding 2-in. dia. cast billets at a temperature of 250°C. This gave a material of 2 to 3 mm. average grain size with a tensile strength of j.400 lb. per sq. in. when tested at a straining rate of 5 per cent per minute. With this extremely soft material, great care was necessary in handling the specimens, to avoid distortion and subsequent recrystallization. The creep tests at 30°C. were conducted in a constant-temperature room, specially built for the purpose in the basement of an office building in which there was no moving machinery, and no vibration was detectable under the most severe conditions of shock in the adjacent surroundings. The room was well insulated and heated electrically, control being by means of a de Khotinsky regulator operating a relay. Maximum temperature variation over a period of several years has been ± 1/2°C. Specimens of the extruded strip, 16 in. long, were used for test purposes with no reduced gauge section, thus eliminating any distortion due to machining. The method of clamping and supporting the specimens is shown diagrammatically in Fig. 1. The gauge marker for the measurement of extension consisted of an aluminum strip, 0.050 in. thick by 0.75 in. wide, one end of which was ground and sanded to a precise knife-edge and fastened to the specimen by suitable pins. After the strip was fastened in place a fine scratch was inscribed just below the knife-edge by means of a sharp teasing needle. Just below this gauge scratch a short vertical mark was made so that the same point could be located and read each time. Several hundred specimens have been prepared by this method, and it was found that with experi-

Jan 1, 1941

By Eric Jette

THE unusual physical, electrical and magnetic properties of the iron-nickel alloys has given rise to a voluminous literature. This work will be reviewed critically in "The Alloys of Iron and Nickel," a monograph of the Alloys of Iron Research Series, soon to be published. In what follows we shall therefore confine ourselves to those of the earlier investi-gations that involved the use of X-ray crystal-structure methods. The earliest X-ray work on the iron-nickel system was by Miss Andrews1. Using the powder method of X-ray analysis purely as a means of identifying the phases present, she located a region between 20 and 30 weight per cent nickel in which body-centered and face-centered phases coexisted. No lattice constants nor details of heat-treat-ment were reported. Bain2 also reported some qualitative observations. McKeehan3 made a systematic investigation over the whole of the system, giving many of his alloys four and some five different heat-treatments. In alloys furnace-cooled from 900° to 950° C. he found two coexisting phases between 0.15 and 30 per cent nickel. The precision of the lattice-constant measurements was low in comparison with what can be obtained today.. Even for alloys of the same heat-treatment, differences in the constants were often between two and ten parts per thousand. In regions where no change of lattice constant with heat-treatment should occur, differences of the same order of magnitude were found. Since the maximum change in the lattice constant of nickel with change of composition is only about 2 per cent of the constant for pure nickel, these variations in the constants for a given alloy cause the points

Jan 1, 1936

By Alfred F. Beasley

The slags derived from the smelting of lead and copper ores are composed essentially of silicates. The problems arising from the smelting of these ores consequently involve the study of silicate fusions. In the absence of specific knowledge concerning the compounds occurring in slags, it has been the practice of metallurgists to treat them in terms of their total chemical composition. Slags have been classified as monosilicates, bisilicates, sesquisilicates, and subsilicates according to the relative amounts of oxygen in the acid and basic radicles of the hypothetical salt produced. While this has been a useful guide to metallurgists in computing the furnace charges, it falls far short of a basis for the scientific investigation of slags. In order to understand the nature of a slag as a whole it is necessary to learn the physical and chemical properties of the mineral compounds which go to make up that slag. The efficiency with which an ore is smelted in a furnace depends primarily on the physical properties of the compounds formed during the operation. When the melting points and fields of stability of each of the mineral compounds in slags have been established, it will be possible to determine the properties of any given slag by examining the nature and amounts of its mineral constituents. Earlier Investigations In 1884 and succeeding years an extensive survey of lead and copper furnace slags was made in Europe by Vogt, and a large part of the present knowledge of the subject is due to his publications.' Vogt's interest in artificial fusions was directed primarily towards the explanation of problems in igneous and economic geology and his subsequent works have been confined wholly to that subject.

Jan 1, 1930

By F. George, W. Tice, M. Salkind

It was found that Al-A13Ni could be readily cold rolled perpendicular to but not parallel to the whiskers. Reductions of more than 98 pct were achieved without cracking by rolling perpendicular to the whiskers, whereas extensive edge cracking was noted after only 15 pct reduction when rolling parallel to the whiskers. The longitudinal and transverse tensile strengths were nearly doubled, and the longitudinal yield strength more than tripled by cold rolling 50 pct in a direction perpendicular to the whiskers. The whiskers exhibited some waviness (elastic bending) as a result of cold rolling, but at very high reductions (greater than 75 pct) whisker fracture and misalignment became significant. A fine dislocation substructure in the matrix consisting of cells attached to the whiskers was pro -duced by cold rolling. Most of- the substructure was readily removed by a 1-hr anneal at 500°C. Cold rolling was found to substantially reduce the thermal stability of the microstructure at 610°C but did not affect the stability at 500°C. FIBER and whisker reinforced composite materials promise significant improvements in properties over conventional materials. Before they find wide use, however, it will be necessary to understand the response of these highly anisotropic materials to common metalworking processes. Most of the nonmetal-lic fiber reinforced materials have very low elongations (a few pct or less) in the direction of fiber alignment. Thus, metalworking techniques such as rolling and forging would not be as broadly applicable to these materials. This investigation was initiated to determine how a composite system consisting of Al3Ni whisker reinforced aluminum responded to rolling, what changes in the microstructure occurred, and the effect of deformation on the mechanical properties. The composite material studied was produced by unidirectional solidification of the A1-Al3Ni eutectic alloy'-7 and consisted of 10 pct by volume of aligned whiskers of Alai in a matrix of aluminum. It should be pointed out that this system is not representative of all composite materials, and the results will therefore not be universally applicable. The A1-Al3Ni system is characterized by: 1) A strong fiber-matrix interfacial bond 2) A ductile matrix 3) A sufficiently low fiber content to allow significant plastic flow between fibers 4) Strong, completely elastic whiskers (tensile strength 400,000 psi, elastic modulus = 20 X 106 psi.1 These factors allow the material to be readily rolled perpendicular to the fibers. If the fiber-matrix bond were not strong, such a weak interface could fail during rolling. A measure of the ability of a composite to be rolled in the transverse direction can be obtained from noting the transverse tensile behavior. In the case of Al-Al3Ni,2 there is considerable ductility (15 to 30 pct). In the case of boron filament reinforced aluminum, for example, the transverse elongation is less than 1 pct,8 and the material could probably not be cold rolled as readily in that direction. EXPERIMENTAL PROCEDURE 3-in. diam ingots of A1-A13Ni eutectic were unidi-rectionally solidified in graphite crucibles. The starting materials consisted of 99.99+ pct pure nickel and aluminum, and the pure eutectic ingots were made with 6.2 wt pct Ni. The unidirectional solidification process (described in detail elsewhere1-3) consists of preparing a master heat of eutectic composition, remelting, and withdrawing the ingot vertically downward through the heat source at a controlled rate so that plane front solidification proceeds upward at a constant velocity. The resulting microstructure consists of 10 pct by volume of whiskers of very high aspect (length to diameter) ratio. The fiber lengths have not been measured because of the difficulty of detecting fiber ends9 but exceeds 104. There is some possibility that the fibers may be continuous within one grain. Flat sheet specimens 2¾ in. sq and approximately 0.2 in. thick containing whiskers parallel to the plane of the sheet and to one edge were used for this study. A1-A13Ni exhibits either a rod-like (high solidification rates) or a blade-like (low solidification rates) whisker morphology,1,3 and both types were studied. Rolling was accomplished using a two-high rolling mill at a speed of approximately 10 fpm. The rolling direction was either parallel to or perpendicular to the direction of growth (direction of whisker alignment). Reductions of from 0.002 to 0.03 in. per pass were used with the most common value being 0.005 in. per pass. Cold rolling of Al-Al3Ni to more than 98 pct reduction in thickness was accomplished with no intermediate anneals. In addition. a series of speci-mens was cold rolled 97 pct with a 1-hr, 500°C anneal in air after each 50 pet reduction. Tensile testing was accomplished using a Tinius-lsen four screw testing machine. Flat sheet specimens + in. wide and between 2 and 2; in. long with the thickness dependent upon rolling reduction, were used. The gage section was in. wide and 1 in. long. Strain was measured using a clip-on LVDT extensome-

Jan 1, 1970