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By Richard E. Gray, Robert W. Bruhn

INTRODUCTION Underground coal mining has been practiced in the United States for over 200 years. Much early mining was not as efficient as today and unrecovered coal pillars, often of variable size and spacing, remain to support the overlying strata after mining has ceased. These conditions constitute a potential subsidence problem since the pillars will eventually fail. The possibility of subsidence above an abandoned mine must be anticipated except when total extraction has been achieved, permitting subsidence concurrent with mining, or when large coal pillars which have an adequate factor of safety for long-term support remain in the mine. Coal is found in 37 states and is mined under- ground in 22 states (HRB Singer, Inc. 1980). Underground mining produced 40 percent of the 7.5 x 10" kg. (830,000,000 tons) of U. S. coal mined in 1980 (Keystone, 1981). There are approximately 70,000 abandoned or inactive underground coal mines in the United States and approximately 2000 active underground coal mines (NAS/NAE, 1975). Underground coal mining in the United States will eventually extend beneath 162 x 109m2 (40 million acres). Thirty-two billion m2 (8 million acres) are already undermined (HRB Singer, 1977). Subsidence due to mining has affected more than 8 x 109m2 (2 million acres) in 30 states, 7.7 x 10 9m2 (1.9 million acres) from bituminous coal mining and the remainder primarily from anthracite mining (Johnson and Hiller, 1979). Subsidence from all other underground mines has affected only 6.9 x 10 7m2 (17,000 acres) (Johnson and Miller, 1979). Subsidence appears to be particularly widespread in two states, Pennsylvania and Illinois, although serious subsidence is found in localized areas of numerous other states (HRB- Singer, Inc. 1977). Host underground coal mining has occurred in the eastern United States, where the U. S. Bureau of Mines estimates 1.6 x 109m2 (398,600 acres) in urban areas in 18 states (out of a total 1.7 x 109m2 1418,400 acres]) are threatened by subsidence (Table 1) (Johnson and Miller, 1979). Pennsylvania and West Virginia contain 57 percent of the total threatened areas. The U.S. Bureau of Mines estimates the total cost to stabilize the estimated 1.7 x lo9m2 (418,400 acres) of subsidence prone urban land located above abandoned mines is over $12.5 billion (1978 costs).

Jan 1, 1982

By AIME AIME

THE Institute of Metals Division of this Institute held a joint meeting with the American Foundry- men's Association on Oct. 5-9, at Syracuse, N. Y. The registration at this meeting was about 150. There were four meetings in all, three of which were in con- junction with the American Foundrymen's Association. This combination works out very nicely and gives the I Division a number of practical foundry papers that it would not get otherwise. The sessions were well attended and the discussion was active. The session on Monday morning was of a general nature and consisted of the following subjects : " Refractory Problems in the Non-ferrous Electric Furnace Casting Shop, " "Temperature Control of Non-ferrous Alloys," "Atomized Coal System of Non-ferrous Melting," "Material Handling in a Brass Foundry." On Tuesday morning, the session was on "Aluminum and Its Alloys." The paper on permanent mold castings created a large amount of discussion, in fact so much that it had to be renewed after the close of the regular program. Aluminum is assuming a more important place every year and adds greatly to the program as a whole. One of the most remarkable meetings that this Division has ever had was held on Tuesday at noon in the form of a Round Table discussion, headed by G. K. Elliott, chairman of the Division, Cincinnati, Ohio. Mr. Elliott divided the members present, numbering about 80, into groups as they were seated at the tables. Each of these groups suggested a topic for discussion. They were as follows : "Fluxes on Market ;" "Simplification of Alloys;" "Pyrometric Control;" "Effect of Gas- sing Metal and Control;" "Barium Sulfate Added to Electric Furnace to Create Slight Oxidation to Remove Aluminum and Silicon;" and" Nickel in Brass."

Jan 1, 1925

By Arnulf Muan, R. E. Johnson

Equilibrium CO2 /CO ratios of a gas phase coexisting with selected oxide phase assemblages of the system CaO-"Fe0"-SiOz and vnetallic iron have been determined at 1080°C. The data obtained are used to calculate activity-conzposition relations for metasili-cute, orthosilicate, and CaO- "FeO" solid solutions, and to determine a new value for the free energy of formation of C&S&0,. The metasilicate solution is practically ideal, whereas large deviations from ideality exist in the othe,r two solid solutions. BECAUSE of the geochemical and metallurgical importance of the oxides CaO, "FeO", and SiOz, the system CaO-"FeO"-SiO2 has been the subject of several experimental studies during the past 30 years. Following the delineation of phase relations at liquidus temperatures by a group of investigators at the Geophysical Laboratory of the Carnegie Institution of Washington in 1933,1 Chipman and associates in the early forties2,3 determined activities of FeO in liquids of this system. Since that time, many attempts have been made to interpret the data of Chipman et al. in terms of the constitution of the silicate liquids and the interaction parameters among the various constituents of the system (see for instance papers by Richardson4 and by Flood and coworkers5). One of the assumptions made in some of these interpretations4 is that the binary silicate systems CaSiO3-FeSiO3 and CazSi04-Fe2SiO4 mix ideally in the solid state. The objective of the present study is to provide experimental data on activity-com position relations in solid solutions of the system CaO-"FeO"-SiO2. Such data will contribute toward an understanding of the thermodynamics of silicate solid-solution phases in general, and will serve specifically to confirm or refute some of the assumptions made in interpreting liquid slag behavior. PREVIOUS WORK Phase relations in the system CaO-"FeO"-SiO2 in contact with metallic iron were determined by Bowen, Schairer, and Posnjak,1 and additional phase-equilibrium data for this system have been presented by Allen and snow.' A reproduction of the most up-to-date phase diagram for this system is shown in Fig. 1.7'8 Of particular interest in the present investigation are the relations among the various crystalline phases slightly below the lowest solidus temperature in the system, as shown in Fig. 2. The present work will be concerned primarily with some of the composition

Jan 1, 1968

By N. A. Gokcen, J. Chipman

A revised treatment of the authors' published data eliminates the complex relation previously proposed between concentration of silicon and activity coefficient of oxygen in liquid iron. Revised values of the thermodynamic properties of the liquid solution are presented. IN a recent experimental study of the reaction SiO2 (s) = Si+ 2O; Kf, = [% Si] [% O]² [1] the authors' found a substantially constant equilibrium product in liquid iron at 1600°C of 2.8x10-5 They also reported extensive data on the reactions: SiO2 (s) + 2H2 (8) = Si- + 2H2O (g); K'2= [% Si] (H2O/H2 [2] and H, (g) + 0 = H2O (g); K'3 =( H2 O [31 (H2) [%O] From the results on reaction 3 and earlier data of Dastur² on this same reaction in the absence of silicon, they determined the activity coefficient of oxygen, f0, on the basis of the definition K3 = (H2O)/ (H2)f0 [% 0] where K, is the equilibrium constant and f0, is taken as unity in the pure Fe-0 system. Similarly values of fsi were deduced from results on reaction 2. In a more recent study" of analogous reactions in the system Fe-A1-0, it was found impossible to reconcile the results on reaction 3 with Dastur's data; accordingly the latter were ignored and the equilibrium results were extrapolated to find a value of K, at zero concentration of aluminum. This procedure failed to locate the cause of the discrepancy but it did yield reasonable values of activity coefficients. It also avoided introduction of the complex empirical relation between the oxygen activity coefficient and the concentration of the added element. The same type of discrepancy exists for system Fe-Si-0.' In the earlier paper an attempt was made to fit both sets of data by a single curved line (Fig. 6 of ref. l), the form of which is contrary to the theoretical requirement of a finite slope at infinite dilution. In the light of experience on the Fe-A1-0 system the discrepancy must be recognized as one which can be resolved only by more refined measurements. Accordingly Figs. 6 and 10 are retracted. It is pointed out also that until the discrepancy is resolved Figs. 7, 8, and 11 are subject to some uncertainty. Qualitatively the following conclusions still appear valid: 1—The activity coefficient of oxygen is reduced by addition of silicon. 2—In dilute solutions the activity coefficient of silicon increases with its concentration. 3—With respect to equilibrium in reaction 1, the above effects are approximately compensating. The discussion of K'1 in the previous paper requires no revision. It was pointed out that the constancy of the product [% Si] [% 0]² ndicated a compensating effect of the activity coefficients of silicon and oxygen. Therefore, as a very good approximation, K1 = K'1 and the following average values are suggested both for K, and K', at the temperatures 1550°, 1600°, and 1650", respectively, 1.0x10-", 2.8~10-" and 5.5 ~lo-'. Revision of the thermodynamic treatment is necessitated by the recent appearance of new data, based on a combination of combustion and solution calorimetry,' which yields for the heat of formation of low-cristobalite from the elements, the value —209,330 ±250 cal per mol at 25°C. This is about 4000 cal larger than the value previously accepted. The new value for cristobalite is used, together with Kelley's tables of high-temperature heat contents" and entropies and with Korber and Oelsen's' heat of fusion of silicon to obtain the following equation for the standard free energy of cristobalite in the temperature range 1700" to 2000°K: Si (1) + 02 (g) = Si02 (crist.); ?F° = -217,700 + 47.OT [4] The free energy of solution of 0, in liquid iron is:8 O2 (g) = 20 (in Fe); AF° = -55,860 - 1.14T [5] and these two equations are combined to give: Si (1) + 20 = SiO, (crist.); AF° = -161,840 + 48.14T [6] ?F°1873 = -71,700 cal. From the experimental value of K, = 2.8x10-5, Si + 20 = SiO2 (crist.); ?F°1873 = -39,000 cal. [7] The combination of Eqs. 6 and 7 yields the free energy change when liquid silicon dissolves in iron to form the dilute solution of unit activity (1 pct). Si (1) = Si; ?F°1873 = -32,700 cal. [8] The heat effect in this process according to Korber and Oelsen' is an evolution of 28,500 cal per gram

Jan 1, 1954

By I. J. Hegyi, J. J. Tietjen, H. Nelson, J. I. Pankove

The fabrication of p-n junctions in GaAsl-,P, alloys by a vapor-phase gowth technique has for the first tirne resulted in room-temperature injection lasers capable of operating over a broad range of wavelengths extending into the visible region of the spectrum. The shortest wavelength achieved to date is 6750A at room tetnperature. In addition, at 78°K the threshold current density values for these lasers are generally the lo~vest reported, and the emitted radiation extends to the lozc,est wavelength ever attained (6350A). With lasers fabricated from material containing 14 pct Gap, quanticm efficiencies of 26 pct and peak power outputs of 25 zu were obtained at room temperature. ALTHOUGH room-temperature operation of GaAs injection lasers has been well-documented,&apos;-5 the operation of GaAsl-,P, (x > 0) laser diodes has been restricted to relatively low temperatures.8-&apos;0 This has been previously attributed5, 7, 10-12 partially to the difficulty of preparing single-crystalline GaAsl-& alloys having a high degree of chemical homogeneity and purity. Also, with these materials it has been difficult to prepare high-quality, abrupt p-12 junctions by diffusion techniques; and, in turn, this has made it difficult to obtain optimum electrical properties for room-temperature operationL3 in the resulting laser diodes. As a result, GaAsl-,P, laser diodes have not been efficient enough to permit operation at room temperature. For example, using diffused structures, only a few diodes were obtained which could be operated even close to room temperature (255K)." Recently, a vapor-phase growth method of preparing epitaxial deposits of GaAsl - .P, alloys has been described,14 and the high-purity and homogeneity of these materials has been previously demonstrated. Of special significance, with this technique, n- or p -type doping can be initiated or discontinued at any time and at almost any rate during the crystal growth so that the donor and the acceptor concentrations can be easily controlled to obtain desired impurity profiles. This permits high-quality, abrupt p-TZ junctions to be vapor-phase grown entirely during the crystal growth process, so that diffusion or other p-n junction fabrication processes are unnecessary. After growth, the device does not have to be heated to elevated temperatures, which avoids the possible unwanted introduction and motion of both impurities and lattice defects. Using the vapor-phase growth method cited above, over 300 room-temperature injection lasers have been prepared from GaAsl-,P, alloys having compositions in the range of 0 5 x 5 0.41. These lasers have emitted cohe~ent radiation in the spectral range of 8350 to 6350A at 78°K or from 9000 to 6750A at room temperature. The threshold current densities of the best lasers are independent of the alloy composition over the range 0 < x < 0.2 and compare favorably with values for good GaAs lasers.&apos; MATERIAL PREPARATION Multilayer, epitaxial deposits of GaAsl-,P, alloys are prepared by a vapor-growth technique described elsewhere.14 With this technique, the individual layers which comprise the multilayer structure are prepared sequentially in the deposition apparatus without interrupting the crystal growth. The epitaxial layers are deposited on GaAs substrate surfaces oriented normal to the ( 100) direction. The substrate wafers employed in this study were usually doped with tellurium to an electron concentration of approximately 2 x 10" per cu cm. To avoid strains, the first 10 to 15 p of the deposited material is uniformly graded from pure GaAs to the specific GaAsl- ,P, alloy composition of interest. The GaAsl - ,P, alloy growth is then continued to form a layer of constant composition having a thickness in the range of 25 to 75 p. Both the graded region and the layer of constant composition are doped with selenium to an electron concentration of about 2 x 10" per cu cm. The p region of the diode is then incorporated in the crystal by abruptly changing the dopant concentrations in the vapor phase to facilitate doping with zinc. This layer has a hole concentration of approximately 3 X 1019 per cu cm and typically is 50 p thick. DEVICE FABRICATION In general, the GaAs substrate and the region of graded composition are removed. Ohmic contacts are made to the n-type side by tin evaporation and to the p-type side by an electrodeless nickel deposition. This is followed by an electrodeless deposition of gold on both sides. The crystal wafer is then cleaved along (110) planes and sawed into rectangular parallelepipeds. Typical dimensions are 100 by 300 for the junction area and 100 µ for the diode height. The diodes are either soldered to a copper stud or pressure-mounted in a copper clip. RESULTS AND DISCUSSION Approximately 400 laser diodes having compositions in the range of 0.41 have been prepared by the method described above. Each laser was routinely tested at liquid-nitrogen temperature. The lasers were operated with l-psec current pulses at a repetition rate of 60 pulses per sec. The parameters of greatest practical interest are the photon energy or wavelength of the laser output and the threshold current density. Fig. 1 shows the variation of photon energy with alloy composition at 78°K. The composition was determined from the lattice constant of the material obtained by X-ray back-reflection measurements. Although there

Jan 1, 1968

By L. W. Reynolds, R. F. Campbell, K. G. Carroll, S. H. Ballard

Based on metallographic and X-ray data probable equilibrium conditions from 1340" to 2400°F are presented for the composition range investigated. These are correlated with investigations of Takei and Kuo. Provision is made for existence of Mo, C and (Fe, Mo)2,C, carbides heretofore omitted in diagrams in this composition range. These carbides and (Fe, Mo),C, in equilibrium with ferrite and austenite, restrict the austenite and austenite + ferrite fields to lower carbon contents and higher temperatures than in the Fe-C system. OK groups of steel of different molybdenum content, but with approximately the same carbon variation in each group, Table I, were studied. The alloys were melted in an acid-lined 30-lb high-frequency induction furnace, and the ingots forged to l-in. rounds, which were then ground to 0.75-in. diam. To minimize chemical segregations a short length of each bar was given a high-temperature heat treatment as listed in Table I. Specimens 0.062 to 0.125-in. thick were thereafter cut from the homogenized bars for heat treatment to determine phase changes in the alloy. Heat treatments were performed in either a lead bath or muffle-type electric furnace, depending upon the temperature required. Maximum temperature variation was * 2" F in the lead bath and * 5"F up to 1900°F and +8"F above 1900°F in the electric furnace. Adequate protection of the specimen from the oxidizing atmosphere in the electric furnace was obtained by sealing the specimen in either a pyrex or a silica capsule which was evacuated or not as circumstances required. For austenitizing followed by quenching to an isothermal temperature, the specimen was placed in a closed-end refractory tube the mouth of which, extending beyond the furnace, was connected to a vacuum pump. The specimen could be withdrawn from this tube and quenched as desired. IDENTIFICATION OF PHASES The principal method of identification of phases was metallographic examination conducted on surfaces well removed from exposure to lead or atmosphere effects during heat treatment. Hardness measurements (Dph/lOkg) were also made on these surfaces. The etching reagents used and their effects are listed in Table II. Martensite and ferrite were readily recognized by their customary appearance after etching with saturated picral or 1 pct nital. The presence of liquid at high temperature was indicated by curved interfaces characteristic of boundaries between solid and melt, by intergranular pools of dendritic areas in a carbide matrix, and by a black network coincident with austenite grain boundaries. Examples of these structures are shown in Figs. l(a) and (0). The types of carbide which were attacked by the electrolytic chromic acid etch and the alkaline KMnO, etch, Table 11, were identified by X-ray analyses of extracted carbides of five alloys. Carbide residue was obtained from a metallographic specimen by etching the specimen for 24 hr in hydrochloric-picric acid in alcohol (grain-size reagent), after which the carbides, standing in relief, were scraped from the surface of the specimen and mounted on a glass slide. Diffraction patterns were obtained with a Philips spectrometer using iron-filtered cobalt radiation. Figs. 2, 3, 4, and 5 illustrate typical etching behaviors with chromic acid and alkaline KMnO,. Chromic acid attacked Mo,C as shown in Figs. 2(a) and (b)-but not (Fe, Mo),C, Fig. 3(b). Alkaline KMnO, attacked (Fe, Mo),C, Fig. 3(c), and also attacked M0,C. In accordance with these behaviors, a typical differentiation of coexisting Mo,C and (Fe, Mo),~ is shown in Figs. 4(a) and (b). The carbide (Fe, Mo),,C, could not be obtained free of other coexisting carbides for etching experiments. The behavior. however. of coexisting carbides identified by x-ray diffraction as Mo,C ind (Fe, Mo),,C, indicate that (Fe, Mo)23C6 is not etched by chromic

Jan 1, 1961

By Alec M. Crowell, C. H. Thigpen

Continuing the increase in production of crude oil and condensate started in 1937, the oil fields of South Arkansas reached a 13-year peak with 26,570,704 bbl. for the year 1942. The stability of the production branch of the industry in the area is demonstrated by Fig. I, which reflects the fact that although the number of producing wells in the state has declined from 3280 in 1931 to 2957 at the end of 1942, total production has continuously increased since the beginning of 1937. This is because all fields discovered since Jan. I, 1937, have observed spacing patterns up to one well to each 160 surface acres, the dual completion of wells where there is more than one producing horizon Eight new pools were brought into production in South Arkansas during 1942 (Fig. 2) They increased the state&apos;s crude oil and condensate reserve by 121,000,000 bbl., bringing the total recoverable reserve figure to 450,000,000 bbl. (Table 3) as of Jan. I, 1943. Abandonment of wells in the stripper areas of the state increased by 32 per cent over the preceding year, there having been 142 wells permanently abandoned in 1942. For economic reasons 279 wells were temporarily shut down as of Dec. 31, 1942. A price increase may start these wells to pumping again and also be the incentive toward the commencing of several secondary recovery projects in the fields discovered between 1922 and 1937. There were 149 wells brought into production in 1942 as against 119 for the

Jan 1, 1943

By C. H. Thigpen, Alec M. Crowell

Continuing the increase in production of crude oil and condensate started in 1937, the oil fields of South Arkansas reached a 13-year peak with 26,570,704 bbl. for the year 1942. The stability of the production branch of the industry in the area is demonstrated by Fig. I, which reflects the fact that although the number of producing wells in the state has declined from 3280 in 1931 to 2957 at the end of 1942, total production has continuously increased since the beginning of 1937. This is because all fields discovered since Jan. I, 1937, have observed spacing patterns up to one well to each 160 surface acres, the dual completion of wells where there is more than one producing horizon Eight new pools were brought into production in South Arkansas during 1942 (Fig. 2) They increased the state&apos;s crude oil and condensate reserve by 121,000,000 bbl., bringing the total recoverable reserve figure to 450,000,000 bbl. (Table 3) as of Jan. I, 1943. Abandonment of wells in the stripper areas of the state increased by 32 per cent over the preceding year, there having been 142 wells permanently abandoned in 1942. For economic reasons 279 wells were temporarily shut down as of Dec. 31, 1942. A price increase may start these wells to pumping again and also be the incentive toward the commencing of several secondary recovery projects in the fields discovered between 1922 and 1937. There were 149 wells brought into production in 1942 as against 119 for the

Jan 1, 1943

By Charles H. Morgan

THE process of wire drawing depends upon the property which certain metals possess, termed ductility, &apos;which is defined in Brande&apos;s Dictionary of Science as a property in consequence of which metals may be drawn out at length without interrupting the continuity of their constituent parts. As defined by M. Tresca, it is the property of flowing when subjected to pressure, and is termed by him the "flow of solids," in his paper, read before the Academy of Sciences in Paris, November, 1865 * In the simple language of the wire shop, it is that quality in certain metals that permit, them to be drawn (or stretched) out through a tapering, hole in a metal block or die, the die being more dense and harder than the metal to be reduced. It is a fact well known to those skilled in the art, that to succeed in drawing iron or steel wire, it is of the utmost importance to have thorough lubrication, as a lack of it would caws abrasion of the wire, or of the walls of the tapering hole in the die or plate, and quickly put an end to the operation. In drawing coarse or large sizes of wire, say 2/10 inch diameter, the pressure upon the sides of the tapering hole, where the wire comes in contact with the die, is so great that an ordinary lubricant is squeezed out when the usual reductions in size are made, and abrasion takes place. In order to meet this difficulty, and secure proper lubrication, it has been&apos; a common practice for years to apply a paste made of rye or wheaten flour, or lime, to the surface of the wire to be drawn, and when the paste is dry, to smear the wire with tallow or grease; the wire is then ready to be drawn, the dried paste serving to prevent the lubricant from being pressed out in the. process. Some years since, when Bessemer metal came largely into use as material for wire, "the writer found that its drawing required so much more power than iron wire, that he was led to institute a series of trials to ascertain the difference in power required. It was found that Bessemer wire required from 100 to 200 per cent. more power to make the same reduction in sizes than soft iron wire, the difference depending upon the amount of carbon and other chemical constitu- * Interesting experiments in the flow of metals have been made, by Messrs. Hoopes Townsend, of Philadelphia, in cold-punching iron, published and illustrated in the Journal of the Franklin Institute, of March, 1878, by Mr. David Townsend.

Jan 1, 1881

By Nicholas J. Grant, H. C. Chang

TRANSCRYSTALLINE fracture surfaces of the cleavage type have been examined by microscopy and X-rays for several metals.&apos; These investigations revealed that the fractured surfaces were not flat and invariably had cleavage and other deformation markings on them. On the other hand, the study of inter crystalline fracture surfaces has been limited. Perryman, in a recently published paper on the inter crystalline fracture of ß-brasses,&apos; found that a thin layer of heavily deformed metal was invariably associated with these surfaces. Furthermore, the thickness of this layer was found to depend on the orientation of the grain boundary surface with respect to the applied stress. The mechanisms of grain boundary sliding and intercrystalline fracture have been presented in two previous papers,which described certain aspects of the deformation of a 20 pct Zn-A1 alloy. It is the purpose of this paper to present some observations on the structure of intercrystalline fracture surfaces and to correlate the structure of such surfaces with the mechanism of intercrystalline fracture. Experimental Techniques—The high purity 20 pct Zn-Al alloy was generously supplied by the Research Laboratories of the Aluminum Co. of America. Two sizes of specimen were used; the first had two parallel flat surfaces of dimensions 1x0.17x0.09 in. and the second was round with a 0.25 in. diam. A grain diameter of 1 to 3 mm was obtained by annealing the specimens at 1000°F for 24 hr. The specimens were then air cooled. The specimens were subjected to creep at 500°F and 2300 psi. The rupture times ranged from % to 3 hr, with one room temperature tensile test. It has been mentioned previous1y" that the intercrystalline fracture surfaces of this alloy, when tested under the conditions given above, are sharply defined. In the optical examination of the fracture surfaces, whenever possible, magnifications of at least X250 were used. The locations of the regions examined, both optically and by X-rays, were selected to give several fracture surface orientations with respect to the stress axis and to the specimen surfaces. This was possible for the X-ray studies since the grain diameters were large compared to the X-ray beam. A film to specimen distance of 3 cm, a 1 mm pinhole and Cr radiation were used for the Laue back reflection pictures.

Jan 1, 1957

By Thirumalai, K.

Although the term "spalling" has long been known, Norton l first referred to its usage for the fracture or disintegration of materials subjected to rapid temperature changes. Spalling of ceramic materials at high temperatures has received attention in the past. Removal of the char formed during ablation in re-entry of space vehicles has been referred to as mechanical spalling. The first experiments to evaluate the process of rock fragmentation by thermal spalling were conducted by Stoces using a series of gasoline burners on the quartz veins of the Zinnwald deep mines in Germany. After the development of rocket-jet burners, the principles of &apos;thermal spalling combined with high fluid momentum found wide practical application in rocks. The well-known jet piercing process for drilling blastholes in taconite and for jet channeling in the quarrying of granite are among the more notable of these application^.

Jan 1, 1970

By C. S. Roberts

Microstructural studies of a Mg-10.3 pct Al alloy showed that discontinuous precipitation during aging multiplies the grain boundary area available for easy deformation in elevated temperature creep. An increase of strain rate for a 6.2 pct Al alloy at 400°F, where precipitation and creep are concurrent, caused an increase in the volume percentage discontinuously precipitated at the completion of the process. The relatively poor elevated temperature creep resistance of heat treated alloys of the Mg-AI-Zn type was explained in these structural terms. C resistance of the heat treatable Mg-A1 based alloys is poor compared to that of Mg-Ce based alloys. While the latter show a continuous precipitate, Mg-A1 alloys prefer a discontinuous precipitate at grain boundaries. &apos;.:&apos; It has been concluded that the excellent creep resistance of Mg-Ce alloys was primarily due to the continuous precipitation which especially localized at the grain boundaries.&apos; The purpose of the present investigation was to obtain a parallel correlation, if such exists, between the poor creep resistance and the state of precipitation in Mg-A1 alloys. Discontinuous precipitation produces about three times as many true grain boundaries as originally existed. This microstructure would be expected to have a marked influence in creep, where quantity of grain boundary area is important. Experimental Procedure The two experimental alloys contained 6.2 and 10.3 pct Al. They were made from electrolytic magnesium by alloying under flux and casting in 3 in. diam permanent molds. The ingots were extruded into 1 1/4 x 1/8 in. flat stock under the following conditions: billet preheat 700°F (2 hr), container and die temperature 700°F, speed 3 fpm, and area reduction ratio 45:1. The creep specimens were machined from blanks which had been solution heat treated 24 hr at 770°F and aged 16 hr at 400°F. Attempts were made to control the grain size as closely as possible for extruded stock. The grain size after solution heat treatment was about two thousandths of an inch for the 6.2 and five thousandths for the 10.3 pct Al alloy.

Jan 1, 1957

L50 Adirondack L1 Alaska L2 Arizona L58 Arkansas L66 Billings Petroleum L3 Black Hills L4 Boston L5 Carlsbad Potash L6 Central Appalachian L60 Central New Mexico L7 Chicago L8 Cleveland L9 Colorado L57 Colorado Plateau L10 Columbia LII Connecticut L55 Dallas L12 Delta L65 Denver Petroleum L13 Detroit L14 East Texas L15 El Paso Metals L71 Evangeline L45 Florida L54 Fort Worth L16 Gulf Coast L61 Hobbs L62 Hugoton L68 Illinois Pet Basin L17 Kansas L18 Lehigh Valley L52 Lou-Ark L47 Mexico L19 Mid-Continent L20 Minnesota L56 Mississippi L21 Montana L22 Nevada L64 Niagara Frontier L23 New York L67 New York Petroleum L25 North Pacific L24 North Texas L26 Ohio Valley L27 Oklahoma City L28 Oregon L63 Panhandle L29 Penn -Anthracite L30 Permian Basin L51 Peru L31 Philadelphia L32 Pittsburgh L33 St Louis L34 San Francisco L59 San Joaquin L35 Southeast L36 Southern Calif L69 Southern Calif Pet L53 South Plains L37 Southwest Texas L48 Southwest Alaska L38 Southwest N Mex L44 Spindletop L39 Tri-State L40 Upper Peninsula L41 Utah L70 Venezuela L42 Washington, D C L43 Wyoming L49 West Central Texas L46 Philippine

Jan 1, 1956

By A. U. Seybolt

In part 111&apos; of this series it was shown that during the selective oxidation of a 3 1/4 pct Si-Fe alloy in damp hydrogen, only silica, (observed at room temperature) as low cristobalite or low tridy-mite or both, was formed as an oxidation product. In some in- „ stances where the film was fairly thin (probably well under 100A) there was some suggestion of an amorphous form of SiO2. The present investigation of oxidation rate showed that the selective oxidation of silicon-iron can be rather complicated, and apparently impossible to rationalize in an unequivocal manner. In some temperature regions, notably near 800" and 1000°C, the data seem to obey the familiar parabolic rate law. However, at intermediate temperatures complications were noted, some of which are possibly due to the order-disorder reaction in the silicon-iron solid solution. IN an earlier report&apos; it was shown that during the oxidation of 3 1/4 pct Si-Fe alloys in H2O-H2 atmospheres only silica films were formed in the temperature range from 400° to 1000°C in hydrogen nearly saturated with water at room temperatures, or at dew points as low as -45°C. In the work to be reported here, some observations are made on the rate of oxide film formation. As in the earlier investigation, electron diffraction patterns generally showed either low tridymite or low cristobalite or both, except for some very thin films. These sometimes showed diffuse rings, presumably due to a very small crystallite size, or in a few cases, diffuse bands probably caused by an amorphous film. EXPERIMENTAL PROCEDURE Vacuum-melted silicon iron made of high-purity materials was rolled into strips 0.014 in. thick, and cut into samples 1/2 in. wide by 1 in. long. Chemical analysis showed 3.2 pct Si and 0.002 pct C. All samples were surface abraded with 600-grit paper, were solvent cleaned, and then placed in an paper,apparatus containing a "Gulbransen type"2 micro-balance. Here the gain in weight of the samples of about 5 sq cm area could be followed as a function of time during the oxidation caused by the water in atmospheres of various controlled water-hydrogen ratios. The water-hydrogen ratios can most easily be described as varying from a dew point of 0°C (PH2O-p^2 = 6.2 x 10-3 , to K (P j -40°C (PH2O/PH^= 1.3 X 10-* Most of the experiments were conducted at the 0°C dew-point atmosphere because drier atmospheres caused so little gain in weight that the accuracy of measurement was poor. Because of this, only the data obtained at PH2O,/P,,,= 6.2 x X3 will be reported. The temperature range extended from 800" to 1000°C; and most of the oxidation runs lasted for about 24 hr. The reproducibility of any reading was about ± 1 ?, but the sensitivity of the balance was about 0.2 ?. The atmosphere, flowing at 200 cm per-min, was preheated to the furnace temperature before contacting the specimen. While the gas flow caused a measurable lift on the sample, it was ordinarily sufficiently constant so that it was not an appreciable source of error. X-ray and electron diffraction checks of the samples before and after oxidation showed no evidence of preferred orientation, either on the metal samples or on the silica films formed. EXPERIMENTAL RESULTS The data obtained are summarized in Table I, and some are given in detail in Figs. 1 to 4. In the fourth column of Table I, kp refers to the parabolic rate constant in the expression (?/cm2)2 = kpt + c [1] where ? = micrograms gain in weight kp = parabolic rate constant in units r2 /cm4 t = time in minutes c = constant It will be noted that in many cases no value for kp is given; this is because in these instances the data did not obey the parabolic rate law. The silica film thicknesses given in the last columns are values calculated from the weight gain, an average tridy-mite-crystobalite density, and by assuming a perfectly plane surface. Fig. 1 shows the data plotted in the form of Eq. [I], hence a linear plot indicates parabolic behavior. It has been frequently observed in the literature that

Jan 1, 1960

By J. O. Brittain, E. P. Lautenschlager, F. Felberbauer

This investigation was undertaken to evaluate the effect of a dispersed phase in a iron upon the strain hardening and the stress dependency of dislocation velocity as inferred from the strain-rate sensitivitv. Experiments were made in a-iron specimens with controlled amounts of carbon and/or A12O3. They were tested at various temperatures between 195&apos; and 373 &apos;K under a variety of conditions oj-concentration, strain rate, and quench aging. The resulting yield strength, flow strength, and strain hardening increased with addition of Al2O3. The parameter m, measured from changes in strain rate, was xsed to describe the stress dependency of the dislocation velocity. m was found to increase with additions of A12O3, increasing carbon in solution, and with increasing temperature. When applied to a recent model for yielding based upon dislocation multiplication and velocity characteristics, the values of m alone did not successfully predict yielding for the materials of this investigalion, but had to be adjusted with a consideration of the number of unlocked dislocations nucleated heterogeneously at discontinuities or inclusions. The change of yield strength with Al2O3 Interpar-ticle spacing appeared to obey a theory of Orowan. EVER since the concept of dislocations has been introduced to explain plastic deformation in crystalline materials, the origin of dislocations and the source of the number of dislocations required to account for plastic deformation have been persistent questions. Ruling out the possibility of homogeneous nucleation,&apos; Gilman2 drew attention to the various cases of heterogeneous nucleation as the source of dislocations, whereas Frank and Read3 introduced the Frank-Read source. However, Gil-man found that the Frank-Read sources did not play a dominant role in the deformation of LiF crystals, but that small precipitates are often, if not always, associated with the nucleation of dislocations. In LiF crystals, however, most of the dislocations arose through the multiplication of moving dislocations in a mechanism described by Koehler4 and Orowan,5 Thus, relatively few precipitates could account for a large number of dislocations. A similar observation of dislocation nucleation at inclusions of precipitates was made by Stein and LOW&apos; on Si-Fe crystals. Their crystals contained

Jan 1, 1964

By Charles Luner

ALTHOUGH the kinetics of the atmospheric oxidation of tin have been studied,1-3 the kinetics in pure oxygen have not been reported. This note presents some results of the kinetics of the oxidation of tin foil in pure oxygen. The tin foil used in this investigation was 99.78 pct pure, the two major impurities being Pb (0.17 pct) and Sb (0.024 pct). The foil was degreased and air-dried prior to oxidation. The air-formed film was estimated by coulometric reduction4 of the surface oxides to be about 25A. The samples, which were in strip form and had a total geometric surface area of about 300 sq cm, were first evacuated at room temperature in an oxidation bulb to 1 X 10 -5 mm Hg and subsequently degassed for 1 hr at the temperature of the experiment. Spectroscopically pure oxygen was then introduced into the bulb. The rates of oxidation were measured by following the rate of pressure change due to oxygen consumption in a closed system, the volume of which was sufficiently large so that the pressure change during an experiment was 10 to 15 per cent of the total pressure. An oil-mercury manometer,5 with a sensitivity of 3 X x mm Hg (which corresponds approximately to 5 X 10 -7 gm of oxygen) was used to measure the pressure change. The oxidation bulb was heated by an oil-bath and controlled to within -10.3 C. The reproducibility of the rates was good, as determined by the coincidence of rates at 190oC for duplicate experiments. Fig. 1 shows the oxidation curves in the temperature range 168 to 211.5oC at 8 mm Hg pressure. The effect of pressure on the rate of oxidation at 190°C is also shown. The rate of oxidation was not markedly affected by changes in pressure in the range 4 to 9 mm Hg, except perhaps at the lowest pressure, 4 mm Hg, where after about 70 min there appeared to be a decline in the rate, as compared with the rate at the higher pressures. At the lower tem- perature, 168oC, and for short reaction times, it is difficult to distinguish between a linear relationship and a slight curvature in the oxidation rate. However, for longer times, there was a somewhat larger indication of curvature. The samples after oxidation were gold-colored in appearance. The oxide that was formed at 170°C was identified as a-SnO by reflection electron diffraction. This is in agreement with results obtained by other workers.6, 7 The rate data best fitted the logarithmic-oxidation rate law, w = K1n ln(1 + -t/to) [1] where w is the weight of oxygen consumed, t is the time, and K In, and to are constants. First estimates to were obtained according to the method of Taylor Thon8 and were then employed to obtain the best simuItaneous estimates of to and K In, that would fit the logarithmic expression. These estimates were found numerically, so that the residual variance could be minimized. The calculations were performed on an

Jan 1, 1961

By Sydney H. Ball

I. INTRODUCTION. DURING the past 50 years the attention of mining-men has been turned to Africa, and within the past decade prospecting-expeditions sent into Central Africa have resulted in the opening-up of several mines. Having recently spent two years in the Belgian Congo for the Société Internationale Forestiere et Miniere du Congo, it is our purpose to outline briefly the mining-conditions in that part of Central Africa. Before it became, in 1908, a Belgian colony, this region was known as the Congo Free State. II. LOCATION AND AREA. The Belgian Congo lies in southwestern Central Africa, west of the continental divide, is illustrated in Fig. 1. It has a coastline of but 20 miles on the Atlantic, but widens rapidly eastward to points 5° north and 14° south of the equator. Its area is 908,000 sq. miles, which is almost one-quarter that of the United States and Alaska, or more than one and one-half times that of Alaska. Stated in other terms, its area is nearly one-third that of the United States, exclusive of Alaska and the insular possessions, or more than that of all the United States east of the Mississippi river. III. TOPOGRAPHY AND DRAINAGE. From north to south, Africa is made up of three topographic elements: 1, the Atlas mountains, a highly-accentuated region

Apr 1, 1910

By Gerald J. Anderson

The Marquette District of Central Northern Michigan is the oldest of the Lake Superior iron districts with a mining history dating from 1852 up to the present. The total production of all types of ore through 1965 was 338,120, 146 long tons. Emphasis up to the 1950's was on mining the direct shipping ores; however, demands for higher-grade and better-structured ores in the last decade has resulted in a complete shift in emphasis to beneficiating the lowgrade Negaunee Iron-formation to produce high-grade iron ore pellets. The Precambrian sediments of the Marquette Range have been correlated with the Animikie Series of the Thunder Bay District, Ontario, and are contained in a westward plunging synclinorium that is approximately 3 3 miles in length and 3 to 6 miles in width. -The rock unit of major economic importance is the Negaunee Iron-formation that reaches a thickness of 2500 feet near the City of Negaunee. The primary iron content of the Negaunee Iron-formation averages 26 per cent, whereas the altered iron-formation approximates 31 per cent. The Negaunee Iron-formation has been divided into three principal types: diagenetic, oxidized, and metamorphic. The ores produced to date fall into four categories: high-grade soft ores, high-grade hard ores, siliceous ores, and concentrates and agglomerates (pellets). The soft ores generally are found in synclines and in fault-trough structures, bounded by mafic dikes along at least one side, and are mainly found in the basal portion of the Negaunee. In contrast, the hard ores occur in the uppermost portion of the Negaunee and are controlled by structural features such as folds, faults, and dikes. Iron-formation that has undergone diagenetic and metamorphic alteration makes up the main beneficiating ore types. Studies on the Negaunee Iron-formation have played an important role in the formulation of many of the theories on the origin of the Precambrian iron-formations.

Jan 1, 1968

By B. A. Wilcox, A. H. Clauer

DURING the course of an investigation on the high-temperature creep behavior of TD Nickel* (Ni + 2) vol pct ThO2), it was observed that the creep fractures were similar in appearance to low-temperature ductile fibrous fractures and creep ruptures by cavitation. Microfractographs of fibrous ruptures are typically characterized by a dimpled appearance, with second-phase particles frequently found near the bottom of the dimples.&apos;-4 These somewhat resemble creep ruptures by cavitation, in that fracture occurs by void formation, with the subsequent growth and final merging of the voids to form a complete fracture.&apos; It is the purpose of this communication to describe the creep fracture of TD nickel and suggest a mechanism for the rupturing process. The discussion is relevant to material crept to fracture in vacuo at a constant stress of 18,000 psi, over the temperature range 900" to ll00°C. The material used in this investigation was 1/2-in.-diam bar stock supplied by Du Pont, contain- ing 2.3 vol pct Tho2. The final fabrication treatment consisted of -95 pct reduction by swaging followed by a 1-hr anneal at 1000°C. Transmission and replica electron microscopy revealed that the material had a fibered structure with a transverse grain size of -1 µ and a longitudinal grain size of 10 to 15 µ. Selected-area diffraction indicated that the fiber axis was parallel to (00l), in agreement with the results of Inman et a1.6 The thoria particle size varied from 80 to 1000Å, with an average size of 400Å, and the mean particle spacing was about 1200Å. The remarkable structural stability7 was confirmed by annealing for 6 hr at 1300°C (about &apos; 0.9 the absolute melting point). Transmission electron microscopy revealed that the only structural change was a slight decrease in dislocation density. Furthermore, recrystallization or grain growth during creep has not been observed. All specimens were annealed in vacuo at 1300°C for 3 hr prior to creep testing. The following times to rupture were obtained for vacuum creep tests at a constant stress of 18,000 psi: 900°C, 854 hr; 930°C,

Jan 1, 1965

By G. R. St. Pierre, A. J. Wilhelem

In connection with the reduction of hematite or magnetite to metallic iron, it appeared desirable to study the rate of reduction of each oxide to the next lower oxide under conditions which excluded all other condensed phases. For this purpose, pellets of Fe,O,, Fe,O,, and oFeOo were prepared. A gas train for the preparation of Ar-Hz-H20 mixtures was employed to establish a continuous flow of a controlled atmosphere over a pellet suspended on a balance. In this manner the following individual reduction steps could be studied: For example, pellets of hematite were reduced solely to magnetite by adjusting the gas atmosphere such that it was oxidizing to wustite. In other words, the reaction was complete when the hematite pellet had been totally converted to magnetite. The pellets were prepared from Baker Chemical ferric oxide. The ferric oxide powder was moistened and handrolled. Air sintering at 950°C produced Fe,0, pellets with a density of 3.65 g per cm3. The pellets ranged in size from 0.6 to 1.2 cm diam. The magnetite and

Jan 1, 1962