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By Arthur Flagg

(New York Meeting, February, 1913.) THE Elk City mining district of Idaho occupies a position near the geographical center of Idaho county, a region of mod¬erate elevation in the western foot-hills of the Bitter Root mountains. The district comprises an area of approximately 350 sq. miles, bounded oil the west by the Newsome district and on the south by the Dixie and Oro Grande districts. There are no mining districts to the north or east. Elk City, the principal town and the seat of the mining office for the district, is situated in a hydrographical basin surrounded by low hills. The elevation is 4,200 ft. above sear level. Through this basin flow Elk Creek, Red river, and American river, which unite west of town to form the south fork of the Clearwater. The one township is set out from the Bitter Root Forest Reserve. Though a railroad starting from the Stites terminus of the Clearwater Short Line of the Northern Pacific railroad has been under consideration for some years, the camp is yet with¬out railroad facilities. The projected road would follow the south fork of the Clearwater on easy grades, but would be very expensive to build and maintain. While such a road would greatly benefit those who are now operating in the camp, and in a slight degree stimulate interest in its possibilities, there is hardly business enough to warrant its construction.

Jan 4, 1913

By D. Jenkins

The Franklin Laboratory was designed mainly for the analysis of the products from the two concentrating mills situated at Franklin and Sterling Hill, the most important determinations being the zinc, iron, manganese, lime, moisture, and silica contents of the ores. Within the last 4 years, however, it has been found advisable to examine most of our supplies, and therefore additional space and equipment was allotted for the examination of such substances as oils, greases, soaps, alloys, fuels, paints, explosives, and water. The building as shown in elevation (Fig. 1) and plan (Fig. 2) consists of a main or routine laboratory, an experimental laboratory, a water analysis room, and the other accessories such as stock room, library, sampling and drying rooms, and office. The main laboratory is further divided into a balance room and zinc analysis room. As the greater part of our determinations are volumetric, good light is a very important factor and with this in view the interior malls of the building were constructed of white enameled brick laid in Keene cement. These also have the additional advantage that they give a clean and attractive appearance to the room. The windows are large, being 76 by 44 in. and even on very dark days the light is good throughout the whole laboratory. Our zinc titration requires a constant light and as, on many days, especially in winter, the light is variable, we installed two Artificial

Jan 1, 1918

By T. E. Weirich

Although 1931 witnessed no new discoveries of oil or gas in Oklahoma, the year is especially outstanding because of price demoralization, political intervention, abandonment of marginal properties, a strict curbing of oil flow from wells in flush fields and an extension of proration into settled fields. In spite of a strict, adherence to proration agreements, the price per barrel of oil sank from 65c to $1.07 to a low level of 10c to 22c. Table 1 gives the price range for crude oil in Oklahoma during the year. Under a martial law order by the governor, a period intervened from Aug. 4 to Oct. 10, of complete shutting in of the flush fields. This condition created an abrupt decline in the production curve during the two months' period. Oklahoma, as elsewhere, is passing through a "transition period" of relieving expensive above-ground storage by maintaining the more copious supplies of crude oil in the natural reservoirs. For many years the thousands of small, nearly depleted wells have been considered as being the "backbone of the industry." A large number of wells of this type are now idle or completely abandoned. More than 1100 abandonments were recorded by the state Corporation Commission during the year. The industry is becoming less interested in these small wells, replacing the former attitude by the curbed potentialities of flush pools. Many of the major companies are grouping these marginal properties with those of adjacent owners, operating the whole

Jan 1, 1932

By R. G. Weavind, R. S. Young, I. Wolf

ONE of the most important fields of investigation at the Diamond Research Laboratory in Johannesburg is concerned with improvements in metallurgical practices for the diamond mining companies, with particular reference to increased recoveries of the smaller industrial stones. Considerable work has been done on the possible application of flotation processes to the diamond industry. From the viewpoint of recovery processes, diamonds in their natural state may be grouped into two classes, the water-repellent diamonds, which adhere to a grease surface, and the water-avid diamonds, which, because of their wettability, will not adhere to a grease surface and must be recovered by means other than the grease tables used for water-repellent diamonds. Experiments in the flotation of small diamonds from both kimberlite and alluvial deposits indicate the following conclusions: Water-repellent diamonds: Satisfactory flotation of —16 mesh diamonds, which are naturally water-repellent, may be accomplished using either Aero-float 25 together with cresylic acid, or Du Pont B23 as frother together with kerosine as auxiliary oily conditioner or froth stiffener. The quantities of reagents required are of the order of 0.15 lb per ton Aerofloat and 0.18 lb per ton cresylic acid. The use of acid circuits is detrimental, and for best results a pH between 7 and 9 should be maintained. R. G. WEAVIND and I. WOLF are with the Diamond Research Laboratory, Johannesburg, South Africa, and R. S. YOUNG, Member AIME, is Director of Research, Diamond Research Laboratory. TN 76B. Manuscript, March 23, 1951. A flotation period of 5 to 10 min is necessary to insure that all floatable diamonds are removed. Diamonds larger than 16 mesh cannot be recovered satisfactorily by flotation. Xanthates do not act as collectors for diamonds, and this is probably associated with their inability to impart a water-repellent surface to this mineral. Water-repellent diamonds smaller than 28 mesh can be floated quite well by the addition of a frother alone, such as pine oil or Du Pont B23. Water-avid diamonds: Partial flotation of the smaller sizes of wettable diamonds can be achieved by preconditioning with fatty acid soaps, cationic amines, and similar reagents, which will impart a water-repellent film to diamonds. Washing to remove excess reagent, followed by flotation, will result in a fair recovery, but the latter is much lower than for water-repellent diamonds. Crushed boart: Recovery of crushed boart from the waste products of industrial uses is best accomplished by first conditioning the diamonds present in the mixture with fatty acids, cationic amines, etc., removing the conditioning agent by washing, and floating in a cell of the pneumatic type. Flotation reagents found to be most suitable are Du Pont B23, and Aerofloat 25 together with cresylic acid. The optimum quantities are 1.2 g Du Pont B23, and 0.55 g Aerofloat plus 1.4 g cresylic acid, per liter of pulp in the cell. A solids-to-water ratio of 1 to 4 is found to be the most suitable, and alkaline circuits are necessary for best results. Diamonds larger than 28 mesh are not recovered satisfactorily by this procedure, but for finer sizes flotation offers an excellent procedure for the reclamation of this strategic industrial material.

Jan 1, 1952

By R. Fawley, M. A. Quader, R. A. Dodd

Stacking fault energies and annealing twin frequencies have been measured for austenitic stainless steels having a) constant 20 wt pct Cr and varying nickel contents, and b) constant 20 wt pct Ni and varying chromium contents. The effect of nitrogen has also been studied and, to a lesser extent, so has the effect of carbon. All measured stacking fault energies plot linearly against the corresponding annealing twin frequencies, suggesting that, for constant prior deformation and grain size, twinning frequency can be used to estimate stacking fault energy. Compositions low in nickel possess the lowest fault energy, while the maximum fault energy within the investigated composition range occurs mound 20 pct Cr-20 pct Ni. Nitrogen has practically no effect on stacking fault energy when increased from 0.005 to 0.05 wt pct, although Planar dislocation glide is associated with higher nitrogen contents; this may be a short-range order effect. Carbon may raise the stacking fault energy a little, and causes pronounced dislocation tangling in deformed alloys. The basically different dislocation structures promoted by nitrogen and carbon, respectively, are not associated with large variations in stacking fault energy, and the reason for the difference remains unknown. INTEREST in the dislocation configurations developed in plastically deformed alloys arises principally from a desire for an understanding of mechanisms of plastic deformation and fracture. Comparatively little basic work has been concerned with austenitic stainless steels, although considerable interest has developed in the fundamental aspects of deformation of these alloys since the suggestion that those compositions deforming essentially by planar glide are particularly prone to transgranular stress corrosion cracking.' Certain facts are well-established. An 18 Cr-8 Ni steel (type 304) has a low stacking fault energy which is increased by higher nickel contents, and the structure of these steels when moderately plastically deformed changes concomitantly from planar to less planar to distinctly tangled dislocation configurations. These changes are thought to relate to changes in stacking fault energy, and considerable effort has been expended in measuring stacking fault energies of austenitic stainless steels through the determination of node curvatures2"4 even though the method has limitations due to formula approximations,5 an upper limit of measurement of 50 erg cm-2 at the most,5 and the necessity of an extremely meticulous experimental technique. Therefore, it is not surprising that only qualitative agreement between different investigators is generally to be found.'-' At high energies where node radius measurements are inappropriate, some use has been made of annealing twin frequencies to estimate relative stacking fault energies, although a recent critical evaluation of the method suggests that it should be used cautionsly with due regard to effects of grain size and prior deformation.6 Finally, there is a question as to whether the structures of some deformed steels are due to ordering effects. In particular, the role of nitrogen in promoting planar dislocation motion has been suggested to be due to ordering,' but similar suggestions have been made for steels having low interstitial contents.4 EXPERIMENTAL Small ingots of austenitic stainless steels (-50 g) were prepared from components exceeding 99.99 pct purity, the nickel and chromium being Johnson Matthey "Specpure" metals. Carbon was added as pure graphite, and nitrogen as CrN. The components were accurately weighed, and it was assumed that the final composition was the same as the nominal composition

Jan 1, 1969

By B. A. Shaw

Historically, microwave tubes have been fabricated from massive metal and ceramic components. The current trend is to lighten tibes for airborne applications. The reqciiremenls of light weight and also reduced cost have created a novel approach to tube structure in which thin-film technology plays a major role. Although the electrical requirements of thin-film circuits in microwave tubes differ from those required or se,niconductor integrated circuits. the technology is basically similar. The stringent requirements of the micvowave tube have created sophisticaled thin-film techniques thut are of interest to the integrated-circuit industry in general. This paper describes a nunzber of thin-jilm techniques recently developed and discusses in detail the application of the technology in microwave tubes. The particular areas of interest are: 1) ceramic mounted thin-film slow-wave structures; 2) thin-film secondary emitters; 3) suppression of tube environnental multipactor by semiconducting' thin films; and 4) age-hardenable and dispersion-hardened thin metal films. SEVERAL thin-film techniques specifically applied to microwave power tubes are discussed in this report. There are two reasons for this work. One is the necessity of reducing weight and cost of microwave tubes and the other is related to overcoming problems in the tube operation by the use of applied thin-film technology. The major emphasis of this work has been on tube slow-wave structures. Other work in the area of secondary emission, either its suppression or its enhancement, is continuing; the most satisfactory results to date have been by utilization of thin-film technology. The requirements of high thermal and electrical conduction together with greater strength than normally obtained with elemental materials have led to the development of dispersion-hardened films. The paper will discuss: 1) ceramic-mounted delay-line microwave tubes; 2) multipactor and secondary emission; 3) hardened films. I) CERAMIC-MOUNTED THIN-FILM SLOW-WAVE STRUCTURES In a conventional crossed-field microwave tube, the slow-wave or delay-line structure is produced from two carefully machined components. One half of the structure is shown in Fig. 1. The other half is the mirror image of the first but is rotationally offset by a half a period. The combined structure now forms an interdigital type of slow-wave structure and is the anode of the tube as shown in Fig. 2. The period and finger length of an interdigital slow-wave structure are prescribed by the desired dispersion characteristics. The typical design is as shown in the first figure; it can be noticed that the finger width is several times greater than the finger thickness. Even assuming that it were mechanically possible to produce free-standing fingers of extremely small cross-sectional dimension, for example, 0.002 in. thick by 0.005 in. wide by 0.500 in. long, decreasing this finger width would increase the tube efficiency but would also decrease the thermal-conduction path, causing an increased temperature rise from intercepted rf current which in its extreme could easily cause finger melting. Hence, for free-standing lines of this type, the design is a compromise between mechanical capabilities, tube efficiency, and thermal dissipation. These structures are also expensive and tend to be heavier than purely electrical considerations would demand. In the present approach, we have transposed the three-dimensional structure previously shown into an essentially two-dimensional structure as shown in Fig. 3. The linear structure is used here for clarity of detail. The support member is a ceramic material and the line is deposited copper. The final tube design is shown in Fig. 4. Because of the backwall sup-

Jan 1, 1967

By T. R. Cass, M. R. Achter

A technique for measuring the creep and rupture strength of nickel specimens bonded by sintered oxide layers has been developed for the investigation of the role of grain-boundary oxide in the oxidation strengthening of nickel during creep at 817 °C. Prom the inverse dependence of the rate of bonding on the thickness of the starting oxide, it is suggested that the rate of diffusion of Ni++ through NiO is the controlling process at the start of sintering. Cornparisons of the creep and rupture strength and of the microstructure of sintered couples with conventionul creep specimens suggest rupture in nickel is prevented by load-bearikzg, ikltergranular layers of oxide. A number of recent investigations have shown that at high temperature and low stress the creep-rupture strength of nickel and nickel-base alloys may be much greater in air than in an inert gas or vacuum.'-7 For example, at 817°C and 2500 psi, nickep failed in vacuum in 48 hr but not in air after 4000 hr, and a Ni-Cr-A1 alloy5 at 1038°C and 3000 psi failed in vacuum in 4 hr but not in air after 731 hr. Fig. 1 is a typical creep curve in air for materials experiencing this pronounced environmental strengthening. A common feature of these curves is the entry into a third stage of accelerating creep, concurrent with the for-

Jan 1, 1962

By Rollin E. Hook, Attwell M. Adair

The yield and fracture behavior of recrystallized chromiztm have been studied in order to gain an understanding of the recrystallization embrittlement-rheotropic recovery phenomenon. The duc tile-brittle tensile transition temperature of recrystallized chromium was found to vary from 225 ° to -80°C as the ratio of specimen diameter/mean planar grain size decreased. The applicability of this observation to other bcc metals is briefly discussed. Brittle fracture in recrystallized chromium was found to be initiated predominately from intercrystalline rupture nuclei. Single crystals exhibit a high degree of ductility at 23 "C. The experimental data indicate that grain boundaries play a significant part in the yield and fracture behavim. Pres training significantly reduces the transition temperature, and high temperature aging does not result in re-embrittle-ment until complete recovery or re crystallization occurs. SEVERAL theories have been used to explain the recrystallization embrittlement-rheotropic recovery phenomenon in chromium. Wain, Henderson, and ohnstone' propose a Cottrell dislocation locking mechanism due to nitrogen, and Weaver and Gross and weaver 3 propose a strain-induced precipitation mechanism involving a chromium nitride precipitate. The researches of many investigators seem to leave little doubt that brittleness in chromium is promoted by interstitial impurities. Smith and seybolt4 have shown that the ductile-brittle transition temperature is lowered as the interstitial content is reduced. weaver3 provides evidence for a 150°C reduction in the tensile transition temperature as the nitrogen content is reduced from 20 to 5 ppm. Maykuth and affee' have suggested that the amount and orientation of grain boundary impurities may be responsible for the brittle nature of recrystallized chromium. This suggestion was based on their findings that wrought iodide chromium possessing a fiberous grain structure is ductile in tension at room temperature while a recrystallized grain structure is completely brittle. Previous investigations have not studied this phenomenon sufficiently to determine its cause. Perhaps this has been largely due to previous experimental findings that brittle fracture observed in chromium has been almost entirely transgranular.' In addition McNeil and imb,' who investigated coarse-grained as-cast chromium, describe the point of initiation of fracture as cleavage, close to the (100) plane, near or at grain bound-daries, or at included particles or voids. However, Hook, Adair, and ipsitt found that fracture in coarse-grained recrystallized chromium is initiated by intergranular rupture and then propagates nearly entirely by cleavage. This result, together with their finding that room temperature ductility in bending is observed for single crystals and coarse-grained polycrystalline specimens for which the number of grains through the specimen diameter is small, suggests that grain boundaries may play an important role in the brittle behavior of chromium. The recrystallization embrittlement problem can be resolved into two questions. These are, whether the controlling mechanism is predominately one of crack initiation or crack propagation, and whether brittle fracture is initiated predominately by slip or twin induced intergranular rupture or by cleavage. The following research was designed to study the role of grain boundaries on the brittle fracture of chromium in an effort to resolve these questions. EXPERIMENTAL PROCEDURES, RESULTS, AND DISCUSSION General Procedure. All tensile specimens (except 0.04 in. diam wires) were prepared from 1/4 in. diam swaged rod fabricated from one ingot. Details of fabrication are given elewhere. The results of impurity analysis for the swaged rod and for the

Jan 1, 1963

By J. G. Y. Chow, S. B. McRickard

The tensi1e properties of Ferrovac iron have been studied from 4° to 300°K. The stress required for macroscopic yielding was found to he constant below approximately 50°K. The effect of mechanical twinning on this low -temperature stress plateau was investigated. The onset of twinning occurs in this iron between 130° and 150°K and depending on its previous thermal history the twinning-stress curue may drop below or remain above the vield-stress curves as the temperature is lowered. Twinning has been shown to initiate slip in quenclzed iron at low temperatures. In no instances, however, did the onset of twinning alter the continuity of the yield stress -tempwature curve. Our data shows that carbon inhibits twinning and slip at low tem-peratures. This observation nay be used to explain the ductile-to-brittle transition in iron. The effect of fast neutron irradiation on yielding and embrittlement in iron and Fe-C alloys is offered as supporting evidence for this viewpoint. THE mode of yielding in iron at low temperatures was studied in an attempt to find an expression based on a single mechanism to describe the thermal dependence of the yield stress of iron. There are two types of inflections observed in the variation of the yield stress with temperature in iron and Fe-C alloys. The first is associated with ductile behavior and consists of a region extending 50" to 100°K above absolute zero in which the yield stress is independent of temperature. The second is observed in more brittle materials such as Fe-C alloys and irradiated iron and consists of an abrupt discontinuity in the yield curve as the temperature is lowered through a ductile-to-brittle transition point. The temperature dependence of the yield stress for iron with four grain diameters as found in this study is shown in Fig. 1. To varying degrees all the curves appear to flatten or approach an asymptotic value as the temperature is lowered below 50°K. Several other investigators1,2 have observed a plateau in the yield stress of iron and steel at low temperatures and in 1956 Louat3 presented a theory which contained an explanation for this behavior. In a subsequent exchange with Erickson and Low4'5 who attributed the plateau to the onset of mechanical twinning Louat8 showed that twinning first occurs in iron and steel tested in tension at temperatures as high as 140°K which is well above the observed plateau in yield stress. Furthermore he pointed out that both twinning and slip are basically dislocation processes and that with modified parameters his original theory still applied when deformation is initiated by twinning. Variables which affect the ductile-to-brittle transition in iron are test temperature, strain rate, composition and grain size.7 LOW,8 Hahn et al.,9 and Hull10 have provided evidence which links brittle fracture at a given temperature with the specimen grain size and the onset of twinning. In fact, Hull equates the brittle fracture stress to the twinning stress. On the other hand brittle fracture has been observed in the absence of twinning and priestnerl1 has given a fracture criterion which is valid whether or not fracture is preceded by extensive twinning. The data presented here clarify the role of twinning in the low-temperature deformation of iron. Strong evidence is given that the amount and distribution of interstitial impurities such as carbon are of

Jan 1, 1965

CHARLES KIRCHHOFF, Chairman. ALBERT SAUVEUR, Vice-Chairman. HERBERT M. BOYLSTON, Secretary, Abbot Bldg., Cambridge, Mass. John Birkinbine, J. Esrey Johnson, Jr., Felix A. Vogel, William H. Blauvelt, William Kelly, Leonard Waldo, James Gayley, . Richard Moldenke, William R. Walker, Henry D. Hibbard, Joseph W. Richards, - William R. Webster. Henry 1%1. Howe, E. Gybbon Spilsbury, Frederick W. Wood. Robert W. Hunt, A. A. Stevenson, The Board of Directors of the Institute has authorized the holding of a meeting under the auspices of the Iron and, Steel Committee in New York City, October 16 and 17, 1913. Gratifying responses have been received to the request of the Committee for contributions, the following papers being already assured: 1. H. M. Howe, Equilibrium Temperature for A, in Carbon Steel. 2. H. M. Howe, The Divorcing of the Eutectoid in Meteorites. 3. H. M. Howe and A. G. Levy, Determination Of the Position of Ae3, in Carbon-Iron Alloys. 4. G. .K Burgess, J. J. Crowe and H. S. Rawdon, Thermal and Microscopical Examination of Professor Howe's Standard Commercial Steels. 5. H. Dl. Hove, Discussion of the Existing Data as to the Position of Ae3,. 6. J. H. Hall, Shock Tests of Cast Steel. 7. H. F. Miller, Jr., The Design of Regenerators for Open-Hearth Furnaces. 8. E. Stütz, Paper on the "Scoria Process." 9. Albert Sauveur, Mayari Steel. 10. Felix A. Vogel, Briquetting. 11. J. E. Johnson, Jr., Paper on " Cast Iron."

Jan 6, 1913

SEC. 1. The membership of the Institute shall comprise seven classes, namely: 1. Members; 2. Honorary Members; 3. Senior Members; 4. Associates; 5. Junior Members; 6. Rocky Mountain Members; 7. Junior Foreign Affiliates. All shall be equally entitled to the privileges of membership, excepting that no member of any class whose residence shall be outside of the United States of America, except those residing in Mexico and Canada, shall be entitled to vote. SEC. 2. Members: A person to be eligible for election or transfer into the class of Member must be at least 27 years of age and must have had at least six years' employ¬ment in the practice of engineering, mining, geology, metallurgy, or chemistry, during at least three years of which he must have held positions of responsibility in one or more of these fields. This shall not apply to Rocky Mountain members. SEC. 3. Honorary Members: Each candidate for Honorary Membership must be recommended by at least ten Members and must be elected by ballot at a meeting of the Board of Directors by the unanimous vote of the Directors present; provided, how¬ever, that the number of Honorary Members shall at no time exceed twenty. Such election shall automatically act as a transfer of such member from any other class of membership to which he may belong. SEC. 4. -Senior Members: The Directors may in their discretion place on the Honor Roll of Senior Members and transfer from any other class of membership other than Honorary Membership the name of any Member or Associate who has reached the age of seventy years and who has paid dues for thirty years, and for good reasons in special cases may vary the age or number of years. SEC. 5. Junior Members: A person to be eligible for election to the class of Junior Member must be qualified through education or experience to hold a subordinate position in engineering, mining, metallurgical, geological or chemical work. He shall be not more than 33 years of age at the time of election. SEC. 6. Associates: A person eligible for election or transfer into the class of Associate shall be one, who, in the opinion of the Committee on Admissions and the Board of Directors, is suitable for such election or transfer by reason of his interest in or connection with mining, geology, metallurgy, or chemistry. SEC. 7. Rocky Mountain Members: Membership in a special class of life member¬ships without annual or other dues and without right to receive the printed literature distributed to other members or the right and privilege of wearing the official badge of technical members, is given to all members of the Rocky Mountain Club at the time of consolidation. These special Rocky Mountain memberships shall be claimable by any member of the Rocky Mountain Club, not already a member of the Institute, availing himself of the privilege within ninety days after mailing of notice to him, by the Secretary of the Institute. SEC. 8. Junior Foreign Afliate: Upon appropriate action by the Board of Direc¬tors and with its approval, members in good standing of any technical society having its headquarters outside of the United States of America, Canada, or Mexico,

Jan 1, 1937

By M. J. Buerger

POSSIBLY the most puzzling features observed during a single-crystal deformation test are the appearance of slip striae on the surface of the crystal and the strengthening of the specimen.1 While the first phenomenon is mainly of theoretical interest, the latter is fundamental to all strain-hardening and cold-working processes in which the deformation occurs by translation. The plastic deformation of crystals has received considerable discussion2 and need not be reviewed here in, any great detail. It has been observed, essentially, that after a certain amount of initial stress is applied, the surface of the crystal becomes covered with sets of parallel striae or rings which appear to divide it into thin slabs or slip blocks.3 The striae are the traces of rational crystallographic planes along which shearing movements are localized, these movements providing the strain which accompanies stress applied beyond pure elasticity. As deformation under the applied stress proceeds the slip blocks shear past one another, although the essentially single-crystal character of the specimen is unimpaired. All of the shearing apparently takes place in the immediate vicinity of the original slip striae without the appearance of new planes of movement.4 Since each increment of strain is attended by an increased stress requirement to continue the deformation, the crystal strengthens during the process.

Jan 1, 1928

By E. S. Bumps

A series of macrographs are presented for the purpose of graphically recording the strain phenomenon that accompanies the energy transition in the Charpy impact testing of a mild steel that is susceptible to strain aging. STRAIN patterns in mild steel Charpy impact specimens were obtained in order to determine whether, on the first appearance of plastic strain during deformation, the initial fracture cracks appear in the region of plastic strain or in the elasti-cally deformed regions between. Although this attempt to locate the initiation of cleavage was not successful, the observed strain patterns illustrating various stress conditions in partially deformed Charpy specimens are presented along with a discussion of the possible dependence of transition energy on the yield phenomenon. Earlier work on the development of strain patterns in mild steel have been reported by Fry1 and later by Jevon.2 Harris, Rinebolt, and Raring3 observed characteristic strain markings on the surface of Charpy V-notch impact specimens fractured above and below the transition temperature which they presented schematically. It is intended that the strain figures presented here will add to the literature a graphic correlation of strain with transition energy in impact specimens. Samples of % in. round hot rolled, 0.20 pct C steel were machined to standard 0.394 in. sq, V-notch Charpy impact specimens. Preliminary testing involved determination of transition temperature, Fig. 1, using a Sontagg impact tester. These data were subsequently used to select temperatures above, within, and below the transition range at which specimens were partially deformed. Partial deformation was obtained by either varying the energy or the testing temperature, see Table I. Macroscopic strain figures shown in Figs. 2 to 19 were produced by several metallographic repolish-ing and etching steps. The macroetchant used was as follows:4 120 g HCl, concentrated; 100 ml water; and 90 g cupric chloride. Strain figures were obtained on the outer surface and on sections through the central portion of the impact specimens in order to determine an approximation of the volumetric strain pattern. In the tensile strain figures reported by Jevon, it was found that strain etching would not work immediately following strain unless the material was heated to 200°C. The impact strain patterns presented here were obtained without this heating, but the specimens were not etched until ten months after straining. This confirms a discussion of Jevon's paper, in which it was pointed out that strain figures can also be developed after aging for long periods of time at room temperature. Hardness of the strained and unstrained portions, revealed by the etched pattern, was explored using R, impressions converted to R, hardness values. Discussion of Results In the impact test, as in the tensile test, some parts of the specimen yield and deform plastically, while other regions are deformed only elastically. The plastic deformation bears a relation to the imposed stress pattern. In the strain figures presented here, the plastically deformed regions are the dark etching ones. The strain figures are always symmetrical because the stress state in the Charpy-type specimen under impact loading is symmetrical. The difficulties encountered to produce initial cracks are intimated in Figs. 2 and 4. At a temperature of —75ºF, the stress was not sufficient to pro-

Jan 1, 1953

By R. Simon, L. Yarborough

This paper presents a correlation for predicting the critical pressures of gas-solvent-reservoir oil systems of the type encountered in gas and solvent injection processes. Experimental data from 14 systems were used to develop the correlation which expresses critical pressure as a function of composition, C7+ mol weight, and C7+ characterization factor. Critical pressures predicted by the correlation for the 14 gas-solvent-reservoir oil systems have an average deviation of 2.8 per cent of the experimental values. The correlation war used to study a wide variety of other hydrocarbon mixtures reported in the literature whose critical conditions are in the range of interest in oil recovery work (100 to 280F and 2,000 to 6,000 psia). Critical pressures predicted by the correlation had an average deviation, expressed as per cent of experimental value, of 5 per cent for 20 miscellaneous mixtures from the literature, and 6.4 per cent for I7 methane-butane-decane mixtures reported by Sage and Lucey. INTRODUCTION Predicting critical points of hydrocarbon mixtures is an important part of phase behavior calculations. If the critical point can be predicted for a specific mixture, the separation between the bubble-point and dew-point regions will be defined, and physical properties of the mixture can be calculated by using the principle of corresponding states. Numerous correlations for predicting critical points of hydrocarbon mixtures have been published. Six of these correlationsl-8 were for light hydrocarbons, and two correlations7,8 ere for high boiling-point petroleum distillates. Organick9 And Eilerts" presented correlations which combined the published data from both light and heavy mixtures, and these correlations became the only available methods for predicting critical pressures for wide boiling range mixtures. In the course of the authors' work on secondary recovery by gas and solvent injection, experimental data were obtained for 14 mixtures of dry gas, ethane-propane-butane solvents, and various reservoir oils. The critical pressures and critical temperatures of these gas-solvent-reservoir oil systems were in the range of 1,900 to 4,800 psia and 180 to 265F. The critical pressures predicted for the 14 mixtures by the correlations of Organick and Eilerts had an average deviation from the measured values of about 13 per cent. The authors felt that it was necessary to develop a better correlation for engineering calculations and the resultant correlation, which is presented on Figs. 1 and 2, predicts the critical pressures of the 14 mixtures with an average deviation of 2.8 per cent. The validity of the correlation was tested by applying the correlation to other hydrocarbon mixtures reported in the literature. This subject is discussed later in the paper. The authors feel that there is also a need for an improved critical temperature correlation for gas-solvent-reservoir oil systems. However, developing a critical temperature correlation is a significant study in itself and is not included in this paper. EXPERIMENTAL DATA The compositions and critical points obtained by the authors for 14 gas-solvent-reservoir oil mixtures are shown on Table 1. The methane concentrations in these mixtures varied from 20 to 63 mol per cent. The intermediate hydrocarbon group, consisting of ethane, propane, and butane, varied from 20 to 64 mol per cent, and the concentration of the C,, fraction from 10 to 20 mol per cent. The physical properties of the C,, fraction covered the range from light, paraffinic, nonasphaltic (Mixtures 5, 6, 7, 8, 9 and 10) to heavy, aromatic, and asphaltic (Mixtures 13 and 14).

By P. Ramachandrarao, T. R. Anantharaman

CONSIDERABLE interest has lately been evinced as regards the nature of chill zones in solidified metals and alloys. Biloni and Chalmersl were the first to show through their study of segregation substructures in some nonferrous alloys that the formation of the dendritic region may be preceded by a diffusionless solidification process, viz., predendritic solidification. Subsequently Bower and Flemings2 tried a special solidification technique wherein the liquid was drawn into a narrow copper mold with polished surfaces and concluded that convection might trigger some multiplication mechanism leading to grain refinement. Using uncoated and partially coated surfaces for molds in the Bower-Flemings technique as well as in conventional molds, Biloni and Morando3 have very recently brought out the importance of the rate of heat extraction on the mechanism of solidification. We report here on the surface structures and substructures observed in a Sn-1 wt pct Pb alloy solidified at even higher cooling rates (riz., l05 to l07 ºc per sec) than those employed by earlier workers. The alloy was made by melting tin (99.99+ pct) and lead (99.9+ pct) in a silica tube under vacuum. Small quantities of the homogenized alloy (0.5 to 1.0 g) were then quenched (or splat-cooled) from the melt by the "gun technique" developed by Duwez et al.4 The thickness of the resultant foils varied from specimen to

Jan 1, 1970

By G. B. Craig, J. Rezek

The critical resolved shear stress of zone-refined zinc single crystals deformed in tension is found to increase with increasing amount of striation substructure. The increase in strength with numbers of striations can be accounted for by a dislocation pile-up mechanism. A somewhat different means of plotting stress-strain data is introduced which allows a more unambiguous choice of yield stress to be made. FEW systematic studies of the role played by mac-romosaic or striation-type substructure in the de- formation of high-purity metal single crystals grown from the melt have been reported. McGrath and Craig' found that striations increased the critical resolved shear stress of zone-refined aluminum crystals, postulating a dislocation blockage by the striations as the strengthening mechanism. Lauri-ente and Pond2 found that, as the etch pit density increased in aluminum crystals grown from the melt, the critical resolved shear stress also increased. Fleischer and Chalmers3 also found changes in the critical resolved shear stress of aluminum crystals grown from the melt at varying rates, but could not be certain whether an increase of strength with rate was due to a higher concentration of impurity in the gage length or to an increase in the number of small-angled boundaries. An early work by Hibbard4 indicated that copper crystals containing lineage boundaries were stronger than those free from this type of imperfection.

Jan 1, 1962

By I. Iwasaki, P. L. De Bruyn

Electrical double-layer properties of the silver sulfide-solution interface in different electrolytes and the influence the properties exert on the adsorption of dodecylammonium acetate (DAA) were studied using an electrochemical titration technique. The flotation behavior of silver sulfide was observed using DAA as collector and the results were correlated with adsorption measurements. Silver and sulfide ions were identified as the potential determining ions and their adsorption densities were measured as functions of the pAg and of the ionic strength at two different pH values. The point-of-zero-charge (PZC) was observed to be at pAg 10.2, the value being independent of pH and of the nature and concentration of the electrolyte used. The surface charge of silver sulfide in these electrolytes was positive for pAg values less than 10.2 and was negative for pAg values greater than 10.2. The adsorption of amine on silver sulfide surfaces at pH 4.7 was found to be strongly dependent on the pAg. A shift in the PZC towards a lower pAg due to the adsorption of amine indicated a specific affinity of dodecylammonium ion towards silver sulfide surfaces. At pH 9.2 a strong adsorption of the undissociated amine molecule was indicated. The PZC shift towards a higher pAg and the adsorption of the amine was virtually independent of the interfacial electrical conditions.

Jan 1, 1972

By Phillip O. Tyree, Joseph W. Mussey

Bio-epigenetic sulphur deposits occur in Pecos, Reeves and Culberson Counties of far West Texas. Sulfate reducing bacteria, utilizing hydrocarbons as energy, transformed gypsum into replacement limestone and hydrogen sulfide. Hydrogen sulfide, retained in the pores of the replacement limestone, was subsequently oxidized by highly oxygenated groundwaters, and native sulphur precipitated. West Texas sulphur was first recognized at surface exposures by William P. Blake, a geologist attached to the Captain Pope Military/ Scientific Expedition of 1854. Attempts were made in the early 1900's to mine these sulphur vent exposures by a retort method, but the ventures met with little success. In 1967, Duval discovered a large sulphur deposit near some of the old sulphur works in Culberson County. Duval also expanded reserves in a small sulphur deposit in Pecos County. The Frasch process, developed for producing sulphur from Gulf Coast salt domes, proved successful in West Texas type sulphur deposits also. However, modifications of the process were necessary to provide economical and efficient sulphur recovery from the varied ore occurrences. West Texas conditions and logistics require the ultimate in productivity to be competitive in the domestic and foreign sulphur markets. Several companies, in addition to Duval, are producing or have produced sulphur in West Texas. As of June 1, 1984, a total of 29.87 million mt (29.4 million long tons) of sulphur had been produced west of the Pecos River. Duval Corporation has produced more than 88 percent of that total.

Jan 1, 1985

By H. I. Aaronson, C. Laird

The kinetics of thickening and of lengthening of ?' plates in an Al-3.93 pct Cu alloy in the temperature range 203" to 300" C were determined by means of transmission electron microscopy. The rate of thickening was found to be less than that allowed by volume diffusion control at all temperatures, by amounts which increased with decreasing temperature, in agreement with the predictions of a general theory of precipitate morphology.1 Thickening was treated on the basis of the ledge mechanism. Ledges were deduced to spread across the broad faces of ?' plates at volume dzjrfusion-controlled rates, as anticipated from the disordered structure of their edges. Lengthening of 8' plates, on the other hand, took Place more rapidly than allowed by volume dzjrfusion. This occurred despite clear morPhological evidence of a bmrier to growth at the edges of these plates. It was concluded that the misfit dislocation structure comprising the barrier requires that lengthening take place by a jog mechanism. The tnisfit dislocations, however, also serve as diffusion short circuits, and allow high overall lengthening rates to be achieved. In Part I' it was shown that, within the range of aging temperatures and times studied, the broad faces of 8' plates formed in Al-4 pct Cu are fully coherent with the a, matrix. Virtually .all of the dislocations present in these faces were found to have developed as a result of plastic deformation in the a phase. Such dislocations are thus "intruders", rather than the more usual misfit-compensating variety. The edges of 8' plates were confirmed, by extension of the earlier studies of Mat-suura and Koda,3 to be made up of edge-type misfit dislocations, in sessile orientation with respect to lengthening of the plates. These interfacial structures should cause 8' plates to thicken and to lengthen at rates less than those allowed under the condition of volume diffusion control, such as would be expected if the interphase boundaries had disordered structures.' The narrow width of 8' plates, the reproducible crystallography of their broad faces, and the appearance of these plates in cross section as octagons rather than as circular discs2 provide qualitative support for these deductions. The present study of the rate of thickening and the rate of lengthening of 8' plates was undertaken in order to examine them on a quantitative basis. I) THICKENING KINETICS OF THE BROAD FACES OF?' PLATES A) Literature Review. The measurements now available on the thickening kinetics of single-phase precipitate plates consist of one plot of the thickening of a proeutectoid ferrite plate in an Fe-C alloy,' showing (as predicted) thickening rates less than those allowed by volume diffusion control. B) Experimental Procedure. Details of the preparation of the 4-3.93 pct Cu alloy used in this study have been previously reported.4 As in Part 1,' transmission electron microscopy was the observational tool employed. A general description of the apparatus and procedures of the electron microscopy studies is given in Section I of Part I. In thin foils, 0' plates tend to form at and parallel to the foil surface.' A direct investigation of the thickening process by means of hot-stage transmission electron microscopy was therefore not feasible. It was thus necessary to use the conventional method of aging individual bulk specimens for a wide range of different times at the various temperatures studied. In each specimen, the thicknesses of a number of plates were measured. Since thin foils prepared from "bulk-aged" material contain a large proportion of grains with orientations near (001) , it was relatively easy to find, near the edges of the foils, the characteristic multifold patterns of intersecting extinction contours which indicate regions where the foil is exactly at an (001) orientation. The thicknesses of large numbers of plates were measured along the (200) branches of the "stars" so that the 8' plates were precisely parallel to the optical axis of the microscope. Wherever possible, intersecting extinction contours were adjusted with the parameter s > 0 to improve the visibility of the plates in bright-field illumination. These precautions, in combination with taking the measurements at the thinnest parts of the foils, minimized the errors in the measurement of the thickness of the plates resulting from inexact parallelism to the electron beam. Since the plates were very thin, it was not easy to measure their thickness on the photographs. The techniques of enlargement and of microdensitometry were employed to minimize errors from this part of the measurement. A further source of possible error, that the plates can appear thicker because of contrast associated with mismatch normal to the plane of the plate, was also considered. The images of the plates were usually thinner than those of dislocations, however, and no anomalous changes in apparent plate thickness were observed when regions of foil containing plates were tilted through various diffracting conditions. Any error from this cause must therefore be small. Other sources contributing errors were: a) the microdensitometer traces per se and the subjective estimates of their peak limits, and b) slight fluctuations in magnification associated with small changes in the current of the objective lens of the electron microscope. The overall error probably amounted to no more than 5 to 10 pct. In order to obtain readily interpretable data on thickening kinetics, it is essential that the diffusion fields of adjacent ?' plates not be allowed to overlap. Calculations'-' showed that this condition is definitely not ful-

Jan 1, 1969

By E. T. Turkdogan, P. Grieveson

The self-diffusion coefficient of oxygen in a liquid silicate slag containing 40 pct SiO2, 40 pct CaO, and 20 pct Al2O3, was determined using the capillary eff;usion technique. Two stable isotopes of oxygen (O17 and O18) were used as tracers. After each diffision run, the slags were reduced with graphite, the evolved carbon monoxide collected and converted into CO,. The oxygen isotope concentrations were obtazned by measuring the (CO2)45/(CO2)44 and the (CO2)46/(CO2) ratios of the gas. It was found that for O17 Exchange of oxygen between neighboring silicate anions, possibly accompanied by the rotation of these complexes, is a probable diffusion mechanism. The exchange of oxygen atoms between holes in the silicate "lattice" may also be postulated. A full understanding of the properties of slags is unlikely unless the structural details are clearly established. Thus properties such as surface tension, viscosity, expansivity, electrical conductivity, ionic mobility, density, compressibility, and so forth, have been studied. Of importance also are the self-diffusion coefficients and the energies of activation for diffusion of the component ions. The self-diffusion coefficients of calcium, 1-3silicon,, sulfur,4 and aluminumS in a ternary silicate slag have been determined with the aid of radio-isotopes. The self-diffusion coefficient of oxygen in such a slag was investigated in the course of the work reported here.

Jan 1, 1962