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By A. P. Herring, M. Hoover, D. W. Fuerstenau

The dissolution of nickel, copper, and cobalt from five different samples of well-characterized deep sea manganese nodules was measured as a function of temperature, pH, leaching time, and particle size. Nickel, copper, and cobalt extraction each respond to these variables in a different manner. The results of this investigation indicate that copper and nickel can be selectively dissolved from iron and manganese at moderately low pH, provided the reaction is given sufficient time. A high dissolution of cobalt with dilute sulfuric acid can only be achieved from nodules that have a low iron content (<5%). The most probable rate-controlling step for copper and cobalt dissolution is diffusion through the pores of the nodules, and for nickel dissolution chemical reaction appears to be rate-controlling.

Jan 1, 1974

By David B. Reger

The expansion of the previously discovered gas pools and an intensified search for additional pools in the Oriskany and deeper sands were the principal petroleum activities in West Virginia during 1941. One small oil pool was discovered and another was considerably extended. One small gas pool was discovered, several isolated well discoveries were expanded into definite pools, and various recognized pools were substantially increased. The proved oil territory of the state was increased about 600 acres and the proved gas territory about 45,000 acres. The new discoveries of oil did not equal withdrawals but gas reserves added were greater than gas withdrawals. Oil activity, as in the past several years, was slight because of unfavorable crude prices. Most operators prefer to leave oil in the ground rather than to drill for it without a better return. Gas activity increased greatly because of better demand, even though the price of gas did not improve. The account of operations, as gathered from trade journals and other reporting services, shows that 838 new wells were drilled, resulting in 114 new oil wells with 2606 bbl. of daily new production; 558 new gas wells with 949,226,000 cu. ft. of daily open flow; and 166 dry holes. Also, 86 old wells were drilled to deeper sands with 9 bbl. and 56,030,000 cu. ft. of added production. On the new wells the oil average was 22.86 bbl. per well per day; and the gas average was 1,701,000 cu. ft. per well per day. On new wells the ratio of dry holes to completions was 13.61 per cent. On deeper drilling to other sands the ratio of failures was 15.12 per cent. From an exploratory standpoint one strictly new oil pool (Higginbotham Run) was opened in Kanawha County and one strictly new gas pool (Lost Run) in Taylor County. One entirely isolated wildcat gave commercial Oriskany-sand gas production and may open a pool. Various other wildcats greatly extended the boundaries of known Oriskany-sand gas pools and various others may have opened new pools in the shallow sands. On the other hand, various Oriskany tests in Harrison, Monongalia, Roane and Wood Counties were dry and all five tests to the White Clinton sand (Sil.) in Boone, Harrison, Kanawha and Wood Counties failed to find commercial production. The principal oil wells completed, by counties, were: Calhoun, 24; Clay, 7; Gilmer, 6; Hancock, 9; Kanawha, 9; Pleasants, 10; and Ritchie, 14. Production for the year was estimated by the Oil Weekly as 3,421,000 bbl., compared with U. S. Bureau of Mines final figures of 3,444,000 bbl. in 1940. The leading counties in gas-well completions were: Boone, 32; Braxton, 19; Cabell, 16; Calhoun, 46; Clay, 20; Gilmer, 37; Jackson, 94; Kanawha, 82; Lincoln, 17; Putnam, 46; Ritchie, 33; Upshur, 20; and Wayne, 33. Production for the year is estimated by the author as 210,000,000,000 cu. ft., as compared to the U. S. Bureau of Mines&apos; final figures of 188,751,000,000 cu. ft.* in 1940.

Jan 1, 1942

By David B. Reger

The expansion of the previously discovered gas pools and an intensified search for additional pools in the Oriskany and deeper sands were the principal petroleum activities in West Virginia during 1941. One small oil pool was discovered and another was considerably extended. One small gas pool was discovered, several isolated well discoveries were expanded into definite pools, and various recognized pools were substantially increased. The proved oil territory of the state was increased about 600 acres and the proved gas territory about 45,000 acres. The new discoveries of oil did not equal withdrawals but gas reserves added were greater than gas withdrawals. Oil activity, as in the past several years, was slight because of unfavorable crude prices. Most operators prefer to leave oil in the ground rather than to drill for it without a better return. Gas activity increased greatly because of better demand, even though the price of gas did not improve. The account of operations, as gathered from trade journals and other reporting services, shows that 838 new wells were drilled, resulting in 114 new oil wells with 2606 bbl. of daily new production; 558 new gas wells with 949,226,000 cu. ft. of daily open flow; and 166 dry holes. Also, 86 old wells were drilled to deeper sands with 9 bbl. and 56,030,000 cu. ft. of added production. On the new wells the oil average was 22.86 bbl. per well per day; and the gas average was 1,701,000 cu. ft. per well per day. On new wells the ratio of dry holes to completions was 13.61 per cent. On deeper drilling to other sands the ratio of failures was 15.12 per cent. From an exploratory standpoint one strictly new oil pool (Higginbotham Run) was opened in Kanawha County and one strictly new gas pool (Lost Run) in Taylor County. One entirely isolated wildcat gave commercial Oriskany-sand gas production and may open a pool. Various other wildcats greatly extended the boundaries of known Oriskany-sand gas pools and various others may have opened new pools in the shallow sands. On the other hand, various Oriskany tests in Harrison, Monongalia, Roane and Wood Counties were dry and all five tests to the White Clinton sand (Sil.) in Boone, Harrison, Kanawha and Wood Counties failed to find commercial production. The principal oil wells completed, by counties, were: Calhoun, 24; Clay, 7; Gilmer, 6; Hancock, 9; Kanawha, 9; Pleasants, 10; and Ritchie, 14. Production for the year was estimated by the Oil Weekly as 3,421,000 bbl., compared with U. S. Bureau of Mines final figures of 3,444,000 bbl. in 1940. The leading counties in gas-well completions were: Boone, 32; Braxton, 19; Cabell, 16; Calhoun, 46; Clay, 20; Gilmer, 37; Jackson, 94; Kanawha, 82; Lincoln, 17; Putnam, 46; Ritchie, 33; Upshur, 20; and Wayne, 33. Production for the year is estimated by the author as 210,000,000,000 cu. ft., as compared to the U. S. Bureau of Mines&apos; final figures of 188,751,000,000 cu. ft.* in 1940.

Jan 1, 1942

By D. J. Dunn, J. L. Huiatt, T. E. Norman

Corrosion studies in laboratory ball mills and grinding environment simulations produce corrision rates and total metal removal rates much lower than those recorded in operating production ball mills. The corrosion component of ball metal loss in many mills probably represents less than 10% of the total loss, judging from AMAX experience and recent US Bureau of Mines (USBM) tests. Such small absolute losses are consistent with ball metal loss measured in production ball mill marked ball wear tests to determine effects of corrosion and abrasion resisting properties of alloys in operating mills. These indicate that metal hardness and microstructure determine relative metal loss rates of a given situation. The combination of ore characteristics and grinding process dynamics determine metal loss severity. Alloying for corrosion resistance and modification of the milling corrosion environment yield relatively small metal loss reductions. Alloying and heat treatment to produce high hardness and microstructures of high carbon martensite and, for cast irons M7C3 carbides, produces the lowest metal losses in typical wet grinding applications.

Jan 1, 1986

By C. L. T. Edwards

In the preparation of this paper, the author has drawn upon experience with the operation of a blast furnace on Ioo per cent scrap burden, which he believes was the first operation of its kind in the country. It is the writer&apos;s further belief that much of the controversy attending discussions of this subject may be obviated by the presentation of a group of facts that should be known by blast-furnace men and open-hearth men alike. The following question has been raised: "Is iron made with scrap in the blastfurnace charge as good iron as that made without scrap—made with straight ore?" This question may he answered in part by the fact that the open-hearth men of the Bethlehem Steel Co. who used pig iron from a blast furnace that operated on Ioo per cent steel scrap found no difficulty in the processing of such iron other than that to be expected from the known analysis. Operation with ioo PeR Cent Steel Scrap During World War I, there was accumulated at the Bethlehem plant of the Bethlehem Steel Co. some 22,000 tons of alloy-steel turnings and borings. This scrap material was highly corroded and, like alloy-steel turnings of that period, were as a drug on the market. There was also a small tonnage of scale, rich in valuable metal. If this scrap could be worked up into pig iron, it would become readily available for use in the open hearth. In order that the pig iron should contain the maximum percentage of nickel, permission was obtained from the Management to try a Ioo per cent scrap operation. Accordingly, a blast furnace was swung over on July 25, 1919; the percentage of steel scrap increased more or less irregularly until July 29, when Ioo per cent steel turnings were charged. Except for occasional charges of nickel scale as an "cxtra," the operation continued uninterruptedly until Aug. 27, when the furnace was swung back to the regular ore—ore and scrap—operation. During this period, the furnace production ranged from a low of 568.60 tons to a maximum of 766.07 tons. At the swing-over from Ioo per cent scrap to the regular burden, the charge I hung up rather severely. While the latter condition has nothing to do with the object of the paper, a brief discussion of the experience will appear later because of the interest it may have for blast-furnace operators. In Table I, results of the first and last days of the ore charge are shown, July 25 and July 29. The last column shows a summary for the period of maximum scrap &apos; charge. The furnace employed had a hearth 16 ft. o in., bosh 22 ft. o in., stock line 15 ft. 6 in., bell 11 ft. 6 in., batter in., bosh angle 73&apos; 27&apos; and a Balrer-Neuman top, with gas-engine blowers. Analyses Range of material charged Gravel: SiO2, 64.40 to 70.54 per cent; A1203, 3.52 to 4.58; CaO, 7.27 to 9.49; MgO, 5.09 to 6.14; FeO, 1.67 to 3.34, ignition loss, 9.50 to 13.83. I

Jan 1, 1942

By C. L. T. Edwards

In the preparation of this paper, the author has drawn upon experience with the operation of a blast furnace on Ioo per cent scrap burden, which he believes was the first operation of its kind in the country. It is the writer&apos;s further belief that much of the controversy attending discussions of this subject may be obviated by the presentation of a group of facts that should be known by blast-furnace men and open-hearth men alike. The following question has been raised: "Is iron made with scrap in the blastfurnace charge as good iron as that made without scrap—made with straight ore?" This question may he answered in part by the fact that the open-hearth men of the Bethlehem Steel Co. who used pig iron from a blast furnace that operated on Ioo per cent steel scrap found no difficulty in the processing of such iron other than that to be expected from the known analysis. Operation with ioo PeR Cent Steel Scrap During World War I, there was accumulated at the Bethlehem plant of the Bethlehem Steel Co. some 22,000 tons of alloy-steel turnings and borings. This scrap material was highly corroded and, like alloy-steel turnings of that period, were as a drug on the market. There was also a small tonnage of scale, rich in valuable metal. If this scrap could be worked up into pig iron, it would become readily available for use in the open hearth. In order that the pig iron should contain the maximum percentage of nickel, permission was obtained from the Management to try a Ioo per cent scrap operation. Accordingly, a blast furnace was swung over on July 25, 1919; the percentage of steel scrap increased more or less irregularly until July 29, when Ioo per cent steel turnings were charged. Except for occasional charges of nickel scale as an "cxtra," the operation continued uninterruptedly until Aug. 27, when the furnace was swung back to the regular ore—ore and scrap—operation. During this period, the furnace production ranged from a low of 568.60 tons to a maximum of 766.07 tons. At the swing-over from Ioo per cent scrap to the regular burden, the charge I hung up rather severely. While the latter condition has nothing to do with the object of the paper, a brief discussion of the experience will appear later because of the interest it may have for blast-furnace operators. In Table I, results of the first and last days of the ore charge are shown, July 25 and July 29. The last column shows a summary for the period of maximum scrap &apos; charge. The furnace employed had a hearth 16 ft. o in., bosh 22 ft. o in., stock line 15 ft. 6 in., bell 11 ft. 6 in., batter in., bosh angle 73&apos; 27&apos; and a Balrer-Neuman top, with gas-engine blowers. Analyses Range of material charged Gravel: SiO2, 64.40 to 70.54 per cent; A1203, 3.52 to 4.58; CaO, 7.27 to 9.49; MgO, 5.09 to 6.14; FeO, 1.67 to 3.34, ignition loss, 9.50 to 13.83. I

Jan 1, 1942

By Y. H. Liu, G. W. Powell

Thin foils made from the gold-rich region of- short (0.15 mm)Au-Ag diffusion couples annealed at 880°C for 1 hr were examined in ax electron microscope and the structures were compared with that of pure gold subjected to identical heat treatments. The couples underwent Plastic deformation (bending) during the diffusional anneal. The foils prepared from the diffusion zone have a higher dislocation density and incidence of subboundaries than pure gold. The plastic bending of the couple can be interpreted in terms of the climb of edge dislocations, which are pavallel to the bend axis, along the direction of diffusion. THE interaction of lattice defects during interdiffu-sion between two metals has been considered by several investigators. In particular, da Silva and Mehl,1 Barnes,&apos; and Bardeen and Herring3 have proposed models based on interactions between point and line defects to account for the Kirkendall effect (marker movement). Each of these models is based on dislocation climb, which can either add or remove lattice planes, induced by an under- or supersaturation of vacancies. A theoretical treatment of the nucleation and growth of voids by the condensation of vacancies has been presented by Seitz.4 Stresses can arise in a binary diffusion couple as a result of the vacancy flux and the gradient in the lattice parameter. rinkmman&apos; has investigated the effects of diffusion-induced stresses on void formation; the results of his analysis suggest that voids can form and grow under the influence of these stresses in the absence of an excess vacancy concentration. The relationships between vacancy supersaturation and diffusion-induced stresses and void formation have been elucidated also by Balluffi and seigle6 who concluded that the stress generated by a vacancy supersaturation aids the growth of voids. Experimental evidence which indirectly shows that stresses are produced by chemical diffusion has been obtained by several researchers.2,7-9 This evidence consists in part of the observation by light microscopy of the formation of subgrains, a process characteristic of the high-temperature deformation of some metals during creep.&apos;0 More striking, however, is the plastic bending of short (0.2 mm) Cu-Ni couples observed by Barnes2 and of boron-doped silicon crystals reported by Queisser.9 Diffusion-induced dislocations in iron and silicon have been investigated by Ainslie et a1.11and Schwutte and Queisser,12 respectively, the former using transmission electron microscopy and the latter an X-ray transmission technique. Matthews and Crawford13 observed the formation of boundaries by the climb of interfacial misfit dislocations in thin, vapor-deposited Au-Pd couples diffused in situ in an electron microscope. In order to obtain additional information on the phenomena associated with defect interaction and diffusion-induced stresses in binary couples, an electron transmission study of foils prepared from the diffusion zone of short Au-Ag couples was undertaken. The initial objective was to investigate the processes occurring at various points of the diffusion zone. Subsequent research demonstrated that foils could be prepared only from the gold-rich region of the diffusion zone using the technique described herein. EXPERIMENTAL PROCEDURE Preparation and Annealing of the Diffusion Couples. The couples were made from annealed, high-purity (99.999 pct). polycrvstalline gold and silver sheets (0.075 mm thick). Shall (0.075 by 5 by 17 mm) elec-tropolished coupons of gold and silver were pressure-bonded by heating the two metals in a graphite device to 770°C and holding at this temperature for approximately 30 min. The quality of the bond was ascertained by metallographic examination at 150 times. Each couple subsequently was annealed at 880°C for 1hr; under these conditions, the extreme portions of the

Jan 1, 1968

By R. W. Shoenberger, J. E. McNulty, B. R. Kuchta, William Spackman, A. A. Terchick, M. E. Hopkins, Norman Schapiro, R. J. Gray, A. F. Duzy, M. P. Corriveau

INTRODUCTION * The United States is fortunate in having abundant reserves of metallurgical-grade coals. Although these coals are better in quality and more accessible than most metallurgical-grade coals found throughout the rest of the world, the best grades of these coals are being depleted. Consequently, more efficient exploration tools and techniques, such as advanced methods of core drilling and logging, correlation by petrography, paleontology, palynology, † physical stratigraphy, and geophysical methods are being used to help assess the extent and quality of the remaining coal reserves. Exploration and assessment of new and existing coal properties become of utmost importance in determining ( 1 ) the economic justification for mining the coal, (2) the optimum design of the preparation plant, and (3) the most effective use of the coal. Recent progress has been made in relating mineral matter, especially pyrite, in coal to geologic conditions and paleogeographic trends. l * Editor&apos;s note: Because of the numerous and varied contributions of the associate authors of this chapter, the text does not differentiate between sections prepared by each individual as has been done in other chapters. † Palynology is the science concerned with plant microfossils, especially spores. pollen. and other fossils of microscopic size.

Jan 1, 1979

By H. F. Bishop, F. A. Brandt, W. S. Pellini

The solidification mechanism of experimental steel ingots (7x7x20 in.) was studied by thermal analysis. It was determined that solidification proceeds in wave-like fashion at rates which are determined by the carbon level, superheat, and mold thickness. The thermal cycles of the mold walls were related to the course of solidification. ESPITE marked advances in the field of solid state transformation, metallurgical research has contributed comparatively little exact quantitative data on the mechanism of solidification of metals. There is, therefore, a great need for such data in the various metallurgical industries. The mechanics of solidification of ingots have been investigated in the past primarily by studies of the rate of skin formation as indicated by bleeding or "pour out" tests. The "pour out" method, however, is a tool which gives only approximate information. In the case of alloys with wide solidification ranges, such as irons and certain nonferrous alloys, the method will not work at all; in the case of alloys of intermediate solidification ranges, such as commercial steels, the information may be misleading. Thus, the general adoption of this method has resulted in divergent conclusions regarding the solidification process. Chipman and Fondersmith1 by means of bleeding tests have shown that the linear growth of a solidifying ingot wall follows a parabola of the general form, D = K C, with the start of solidification delayed until superheat is exhausted, as indicated by the constant C. These tests were carried only to a wall thickness of about 5 in. using an ingot of approximately 17x39 in. in cross-section; hence the latter stages of solidification were not studied. Matuschka2-3 indicated that linear solidification of ingots is rapid at first, then slow, but toward the end of solidification the rate becomes extremely rapid again. Spretnak&apos;s4 bleeding studies indicated that, wall growth is expressed more rigorously by two parabolas, and that their point of intersection corresponds to a change of solidification mode from columnar to equiaxed. Spretnak also showed that the K values of the first parabola are always the same regardless of superheat. Nelson bled ingots of square cross-section and found that linear wall growth is initially rapid but decreases continually until the end of solidification. He also concluded that rate of solidification in ingots of square cross-section increases 2.15 pct for every 10 pct increase in cross-sectional area of the mold. The mold ratios considered (ratio of cross-sectional area of the mold to cross-sectional area of the ingot) were all less than 2 to 1. The subject of solidification has also been treated mathematically in many cases, but because of the lack of accurate thermal constants and the simplifying assumptions required, as their authors generally acknowledge, they represent only approaches to the actual conditions of ingot solidification. A third method of studying solidification is the electrical analogue method promulgated by Pasch-kis6-7 and by Jackson and coworkers.8 This method treats solidification as a heat transfer problem with the solidification cycle synthesized on an electrical circuit. Paschkis in his treatment of solidification considered the fact, which was generally ignored, that solidification of steel is not simply the growth of a plane solid wall but a more complex process occurring over a temperature range as indicated by the constitution diagram. Undoubtedly, the anomalous results obtained by bleeding tests arise from the inability to measure quantitatively this mushy condition. The shape of Paschkis&apos; solidification curves are more nearly in accord with those of Matuschka, in that they indicate rapid linear solidification at the beginning and end of solidification with intermediate solidification occurring at a slower rate. Paschkis indicates a definite lengthening of solidification time with increasing superheat. Thermal analysis is a direct method providing exact information for all types of metals regardless of solidification range and was thus adopted in the present program to follow the entire course of solidification from the surface to the centerline of the ingots. The method has the added advantage of being adaptable to following the thermal cycle of the ingot mold during the course of solidification. Test Methods The ingots studied were of square cross-section, 20 in. long, tapered from 71/4 in. at the top to 63/4 in. at the bottom, and fed with a hot top 7 in. in diam and 12 in. high. The molds were uniform in wall

Jan 1, 1953

By R. L. McCarron, G. R. Belton

The diffusivities of oxygen and sulfur in liquid iron have heen determined hy a capillary technique in which the surface concentrations of the solutes were established by means of appropriate H2/H2 and H2S/H, gas mixtures. Total diffusate and concentration profile results are shown to be in good accord, yielding for- 1560 and Supporting results at 1660°C are also presented. The conditions necessary to avoid gas transport control in this type of experiment are discussed. IN spite of their importance in understanding the kinetics and mechanisms of refining reactions, the dif-fusivities of oxygen and sulfur in liquid iron are not well established. Accordingly, as a first step in studies of rates of solute absorption from the gas phase into liquid iron, new measurements of these diffusivities have been made and are presented in this paper. The only published results for the diffusion of sulfur in pure liquid iron are those of Kawai.&apos; He used a diffusion couple technique in which two cylindrical specimens, one containing sulfur and the other with negligible sulfur concentration, were joined together and held in a refractory capillary. After an experiment, the sample was quenched and the concentration distribution of the solute determined. Kawai recognized that significant changes in solute distribution occurred during melting and freezing and he attempted to correct the concentration profiles for these effects to give a sulfur diffusivity of 4.6 x 10-6 sq cm per sec at 1560°C. The method of correction, however, was not rigorous and the uncertainty in this result cannot be easily assessed. Koslov et a1.2 have reported the diffusivity of oxygen in iron as 7.8 x 10"3 sq cm per sec at 1660°C. This value appears to be unreasonably high but, unfortunately, details of their experiments are not available. Shurygin and Kryuk have used the rotating disc method for a study of oxygen diffusion in liquid iron. In their experiments a silica disc was rotated in liquid iron containing oxygen, and the rate of formation of liquid iron silicate was determined by measuring the decrease in weight of the disc. On the assumption that the rate of dissolution was controlled by the diffusion of oxygen in the iron, the diffusion coefficient was computed to be 5.2 x sq cm per sec at 1550°C. However, the Levich equation, which was used to interpret the rate data, was originally de- rived for the case of mass transfer between a solid disc and a single-phase liquid. The hydrodynamic and diffusion boundary layers in the iron stirred by a disc, via coupling of the silicate melt, may be appreciably different from those predicted by Levich&apos;s equations. Recently, Novokhatskiy and Ershov, using an identical experimental method to that of Shurygin and Kryuk, obtained a diffusivity for oxygen in liquid iron of 1.22 x 104 sq cm per sec at 1550°C: no reasons were offered for the disagreement. Schwerdtfeger5 has also recently studied the diffusivity of oxygen in liquid iron. He reacted shallow melts of liquid iron, 0.5 to 1.0 cm deep and contained in high-purity alumina crucibles, with appropriate H20-HZ-He mixtures. The total sample was analyzed, without sectioning, to obtain the average concentration of diffusate. A value at 1610°C of D = 12(3) x 10-5 sq cm per sec was obtained from the results of twenty experiments.= Oxygen profile measurements, which were carried out in three additional experiments using long capillaries and the semiinfinite boundary conditions, indicated a diffusivity about half that computed from the shallow bath experiments. Possible sources of error in Schwerdtfeger&apos;s study will be discussed later in this paper. EXPERIMENTAL TECHNIQUE The essential arrangement of the diffusion cell is shown in Fig. 1. The liquid iron was contained in an alumina capillary, 3 to 4 mm diam and 3 to 9 cm long, which was supported by a hollow alumina pedestal and this whole assembly was held within a movable alumina reaction tube. This tube, which was about 7 mm in bore

Jan 1, 1970

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

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

Jan 1, 1965

By J. Leja, N. Sheikh

The stability of lead ethyl xanthate precipitate in aqueous environment of different pH (4.5 to 10.5) and at temperatures 25°C-60°C was investigated. Dissolution leads to a wide variation of pH, xanthate, and lead ions concentration in solution and to a deposition of solid products of reactions. X-ray diffraction patterns of these solids enabled identification of Pb(OH)3, PbCO3, and PbS as constituents of the remaining undecomposed Pb(EtX)1, together with some unidentified compounds (which give rise to intensive peaks with d values of 2.82A and 1.71A, and numerous peaks of lesser intensity).

Jan 1, 1974

By M. J. Pool, P. J. Spencer, J. R. Guadagno

THE present work was carried out as part of a general program to study the magnitude and concentration dependence of exothermic heats of solution of various metals in liquid tin. Thermodynamic data for the Te-Sn system are very limited, particularly for dilute alloys. Indeed, apart from the prior heat of solution determinations of Pool,1 the only other published values are those of McAteer and seltz2 who carried out electromotive force measurements on solid alloys of compositions from 75 to 95 at. pct Te at temperatures between 543° and 668° K, of Colin and Dro-wart3 who made mass-spectrometric studies of the vapor in equilibrium with solid SnTe, and of Robinson and Bever4 who determined the heat of formation of SnTe by solution calorimetry. The present work thus provides further thermodynamic information for this system, specifically in a temperature range where the solubility of tellurium is very limited. The liquid metal solution calorimeter used in this investigation has been described previously.&apos; No further discussion of its design or operation will therefore be given here. For each series of measurements a tin bath consisting of approximately 70 g of 99.99 pct pure Sn was carefully weighed out and inserted in the calorimeter which was maintained at the desired temperature to within ± 1/4°c. Tellurium, of 99.999 pct purity, was supplied by Atomergic Chemetals Co., a division of Gallard-Schlesinger Chemical Manufacturing Corp. Approximately 0.0006 to 0.001 g-atom specimens of tellurium were used for each experimental run and these were added to the calorimeter from a temperature of 273" K. Heat of solution values were calculated by analysis of a strip-chart recorder plot of the heat effect accompanying the solution of each sample in the tin bath. The heat capacity of the latter was determined at regular intervals during a series of tellurium drops by using pure tin or tungsten calibration samples, the heat contents of which were obtained from the standard compilation of Hultgren et al5 The composition of the bath was calculated after each drop from a knowledge of the weights of tin and tellurium added. Values of the heat of solution of tellurium at 725" and 775° K are listed in Table I together with the corresponding tellurium contents of the alloys. The data are also plotted as a function of tellurium concentration in Fig. 1, which includes the equivalent data obtained by pool&apos; at 750° K. It can be seen that the heat of solution remains

Jan 1, 1969

By Alfred Weiss

The Daniel C. Jackling Award, established in 1953, is presented for significant contributions to technical programs in mining, geology, and geophysics. This year&apos;s recipient, Alfred Weiss, was cited "For his pioneering achievements in applying systems analysis, operations research, and computer methods in exploration, mining, and environmental control; and in disseminating the new technology to the worldwide mining community; and for his lecture, “New Concepts and Tools in Decision-Making.”

Jan 1, 1979

By J. Handin, S. J. Bauer, M. Friedman

Deformation mechanisms in room-dry and water-saturated specimens of Charcoal Granodiorite, shortened at 10-4s-1, at effective pressures (Pe) to 100 MPa and temperatures to partial melting (?1050°C) are documented with a view toward providing criteria to recognize and characterize the deformation for geological and engineering applications. Above 800°C strength decreases dramatically at effective pressures ? 50 MPa and water-weakening reduces strength an additional 30 to 40% at Pe = 100 MPa. Strains at failure are only 0.1 to 2.2 percent with macroscopic ductility (within this range) increasing as the effective pressures are increased and in wet versus dry tests. Shattering (multiple faulting) gives way to faulting along a single zone to failure without macroscopic faulting as ductility increases. Microscopically, cataclasis (extension microfracturing and thermal cracking with rigid-body motions) predominates at all conditions. Dislocation gliding contributes little to the strain. Precursive extension microfractures coalesce to produce the throughgoing faults with gouge zones exhibiting possible Riedel shears. Incipient melting, particularly in wet tests, produces a distinctive texture along feldspar grain boundaries that suggests a grain-boundary-softening effect contributes to the weakening. In addition, it is demonstrated that the presence of water does not lead to more microfractures, but to a reduction in the stresses required to initiate and propagate them.

Jan 1, 1982

By James E. Howard

At the request of the Council of the Institute, I have the honor to submit the following remarks upon the Program of Tests under which the current work of the Watertown Arsenal Testing Laboratory is carried on, which comprises, among other items, the tests of steel ingot metal and derivative shapes. The intended scope of the tests may be illustrated by extracts from the descriptive part of the program as submitted by the Laboratory under date of April 17,1907, and subsequently approved by the Chief of Ordnance, U. S. A. Under Item 1, Ingot Metal—Open hearth, acid and basic; Bessemer, acid and basic; crucible; fluid compressed and uncompreesed—descriptive remarks were made as follon-s: "A thorough, fundamental inquiry into the physical properties of steel necessarily begins with the ingot metal. Investigations, having for their object the improvement of steels, should also begin with the ingot. A knowledge of the ingot structure is essential for judging of the subsequent behavior or appearance of the metal. Under ordinary conditions, so little information is obtained from the ingot in individual cases that practically none of importance is acquired. These remarks have particular reference to the state of physical and structural

Jan 1, 1909

By S. R. B. Cooke, R. O. Huch, C. S. Chang

IN the flotation of iron ores laurylamine derivatives have been used for considerable time.1, 2&apos; To effect satisfactory separation of the gangue, pre-dominantly silica, from the iron oxide minerals, the addition of specific depressants for the iron oxides has been found necessary. Starches and starch products have been used for this purpose.V here is, however, very little published information on the effects of these materials and other variables on this process. In some cases it has been found that prior acid scrubbing and desliming are essential," and depending upon the efficiency of the subsequent washing step, there will be accompanying changes in pH. It was the object of this investigation to test and observe the effects of the above factor as well as to examine and compare the action of various starches and starch products. Ore Preparation The ore used in this experiment was a wash-ore tailing obtained from the western Mesabi range. Microscopic examination and x-ray analysis of the ore showed it to consist of hematite, goethite, and quartz. Physical properties of the iron minerals ranged from hard and crystalline to earthy and ocherous. The quartz grains were discolored either because of iron-oxide inclusions or because of a sur-face coating of iron oxide. The ore assayed 27.52

Jan 1, 1954

By William Y. Holland, Roger H. Cook

Dexter H. Reynolds (Chapman and Wood, Mining Engineers and Consulting Geologists, Albuquerque, N. M.)—A number of questions are raised by conclusions and inferences made in the above-mentioned paper. The more troublesome of these concern use of the various pozzolans to combat the deleterious effects of the alkali-aggregate reaction. The most alkali-reactive materials listed are opal and rocks containing opaline silica. The pozzolans mentioned specifically for use as amelioratives are opaline shales and cherts. These are stated to retard the expansion caused by the alkali-aggregate reaction. Another well-recognized pozzolan is diatomaceous earth, which consists principally of opaline silica. A pozzolan presumably owes its effectiveness to its high reactivity with the alkaline liquid phase of the concrete mix. It appears reasonable to expect that finely divided opaline silica added as a pozzolan would be more susceptible to reaction with the alkalies present than would larger particles of the same material. The authors report that work with high and low alkali cements indicates that in the presence of alkali-reactive materials, deleterious expansion depends upon the alkali content of the cement. The total effect, therefore, should be more or less independent of the amount of reactive aggregate present, and still more independent of its state of subdivision. The deleterious effects should, if anything, be aggravated by the addition of a finely divided, highly reactive pozzolan. Further, if the alkali-aggregate reaction is of great importance in the long-term soundness of concrete structures, the addition of a pozzolan to a concrete made with aggregate free from known deleterious materials would be a questionable procedure. The benefits reportedly accruing from such use of pozzolans are greater ultimate strength for a given cement content, increased resistance to deterioration by exposure to sulphate solutions and other mineral waters, and greater resistance to damage by wetting and drying and freezing and thawing. In view of the deleterious effects of highly reactive materials are these benefits ephemeral? The same considerations apply to another alkali-reactive material, chalcedony, which appears to consist of ultrafine-grained quartz, with opal absent in detectable amounts. Quartz flour is notably reactive chemically and physiologically (cf. Ref. 11 of Holland and Cook&apos;s paper), a fact borne out by its effectiveness as a pozzolan, which presumably might be expected to offset the deleterious effects of the presence of chalcedony in the aggregate. A second question of some importance concerns the reportedly highly deleterious reactivity of acidic and intermediate volcanic glasses, such as rhyolite, perlite, and pumice. Air entrainment is listed as one of the ameliorative measures to combat the deleterious effects of the alkali-aggregate reaction. The alkalic-silica gel formed by the reaction may expand into air bubbles and thus not cause appreciable expansion of the concrete mass. It would appear then that pumice and perlite, particularly perlites of the pumiceous types and other types after expansion, would also tend to counteract the expansion, since these materials consist largely of voids and air bubbles. Certainly this would be expected of structural concrete in which pumice or perlite is used as total aggregate. Finely ground pumice, perlite, and volcanic ash have been demonstrated to be active pozzolans (cf. Pumice as Aggregate for Lightweight Structural Concrete by Wagner, Gay, and Reynolds, Univ. of New Mexico Publications in Engineering No. 5, Albuquerque, 1950). In fact, the term pozzolan was first associated with finely divided pumice or volcanic ash. Such materials were used with hydrated lime as the sole cementitious agent in constructing public buildings, roads, and aqueducts by the ancient Romans. The deleterious alkali reactivity of the volcanic glass, itself containing several percent of the alkalies, apparently did not contribute to the remarkable state of preservation of those ancient structures, as exemplified by the Appian Way and the Pantheon Dome. Still a third question involves .the reactivity of constituents of concrete when exposed to various salt solutions. Resistance to. deleterious expansion and cracking as a result of contact with mineral waters and its relationship to the mineral content of the aggregate are not mentioned by the authors. Yet the phenomena pictured in Fig. 1, and especially in Fig. 2, appear very much like those caused by exposure to mineral waters. The deterioration of concretes exposed to sulphate waters is generally considered related to the chemical constituency of the cement itself, particularly to the relative amount of tricalcium alum-inate contained. Could not many of the ill effects presently blamed on alkali-aggregate reaction really have been caused by contact with sulphate or other salt-containing mineral waters? Or perhaps their use as mixing waters? May not the deleterious expansion be as much a function of the chemical makeup of the cement as it is of the mineral constituency of the aggregate? Would it not be just as important to use alkali-free mixing water as it is to use a low-alkali cement? It appears obvious that resistance of cements and concretes to sulphate and other salt solutions cannot be left out of account in discussion of deterioration of concrete structures with time. This factor may be of equal or even greater importance than the alkali-aggregate reaction, particularly for concrete subjected to wetting and drying cycles, such as airstrip paving, water-retaining dams, and highway structures. Another very important factor is called to attention on page 1022 of the article in Mining Engineering, October 1953, in that failure of concrete structures may result from poor construction practices and use of too high water-cement ratios. Both of these can contribute remarkably to decreased resistance to attack by sulphate waters, and presumably could have an equally remarkable effect upon extent of damage resulting from the alkali-aggregate reaction. From the above remarks it appears that while alkali-aggregate reaction may be an important factor in decreasing the useful. life of a concrete structure, it is not the only factor involved, and it may not be even a controlling factor. Likewise, many of the phenomena apparently associated with the alkali-aggregate reaction may have resulted from cond&apos;itions which had little relationship to the alkali-reactivity of a constituent of the aggregate. Certainly if alkali-aggregate reactivity is a major factor in bringing about early failure, one cannot help feeling anxiety concerning the future of the many concrete structures in this country and abroad in which pumice and perlite were used as total or partial aggregates. This anxiety can only be dispelled by calling to mind that among the best-preserved relics coming down to us from ancient times are structures made with mortars containing highly alkali-reactive aggregates.

Jan 1, 1955

By R. W. Smith, M. E. Brookes

The temperature at which th: quenched 0&apos; (ordered bcc) phase transfo.rms to the ( (complex hexagonal) phase on heating has been examined for certain Ag-Zn and Ag-Au-Zn alloys using an electrical resistivity method. The transition temperature decreases by approxinzately 7°C as the zinc content is reduced by 1 at. pct. The critical temperature, Tc, for long-range order has also been measured for a number of Ag-Au-Zn alloys. Extrapolation to zero gold content suggests that Tc decreases by approximately 5°C per 1 at. pct reduction in zinc content. The 0 phase of the Ag-Zn system exists over a narrow range near the composition Ag zn,&apos; Fig. 1, and has a bcc structure which is disordered above 272°C. Slow cooling to temperatures below the range 274"/258"C allows the complex hexagonal phase, r° to form.2 This is the stable structure at room temperature.3 Upon quenching 0 -phase alloys from high temperatures, it is found that the 0 — (&apos; transformation is suppressed; but ordering takes place (i.e., 0 -0&apos;). This ordered structure can also be obtained by the room-temperature aging of cold-worked (0.4 Deformation of the 0&apos; phase gives rise to a fur- ther hexagonal phase ( (of nearly ideal axial ratio) which reverts to b&apos; within a few hours.= In view of this, it has been suggested that the equilibrium struc-

Jan 1, 1969

By Robert E. Green, Wolfgang Sachse

Simullaneous ultrasonic attenuation measurements of both quasishear waves propagating in single cryslals of aluminum indicate that, in the undeformed annealed state, the dislocation density is generally not uniform on all slip systems. Change oof attenuation measurements made during plastic defortnation of crystals , which possessed specific orientations ideal for studying the orientation dependence of dislocation damping, indicate that, for low strain levels, dislocation motion occurs on additional slip systems besides the primary one, even for crystals oriented for plastic deformation by single slip. THE sensitivity of internal friction measurements permits such measurements to be used successfully in studying the deformation characteristics of metal crystals. On the basis of experimental observations, T. A. Read1 was the first to associate internal friction losses with various dislocation mechanisms. Since that time further work2-&apos; has been performed and a dislocation damping theory has been formulated by Granato and Lucke.6 In the amplitude independent region, this theory predicts the attenuation a to be dependent on an orientation factor O, a dislocation density A, and an average loop length L. if is a constant, independent of crystallographic orientation. For a given crystallographic orientation, changes in dislocation density and loop length give rise to the observed attenuation changes accompanying plastic deformation. The Granato-Liicke theory suggests the investigation of the orientation dependence of attenuation measurements in hopes of obtaining information to separate dislocation motion losses from other losses.7 An experimental study of the orientation dependence of attenuation in undeformed annealed single crystals should yield an insight into the uniformity of dislocation distribution throughout the entire specimen. A similar study on crystals plastically deformed in a prescribed fashion should give information about the alterations in the dislocation distribution on the slip systems activated during plastic deformation. The possible modes of elastic waves which can be propagated in aluminum,8 copper,9 zinc,10 and other hexagonal metals" have been calculated. Associated with each mode of wave propagation are dislocation damping orientation factors, which are based on the resolution of the stress field of that particular elastic wave onto the various operative slip systems in the material. These orientation factors have also been calculated as a function of crystallographic orientation in the papers cited above. Einspruch12 obtained agreement between predicted and observed attenuation values of longitudinal and shear waves in (100) and (110) directions of two undeformed aluminum crystal cubes. He ascribed the slight deviations between predicted and observed values to a nonuniform dislocation distribution, or to other loss mechanisms. In shear deformation of zinc crystals, Alers2 found that the attenuation of shear waves having their particle displacements in the slip plane was very sensitive to the deformation, while the longitudinal wave attenuation was affected only when the wave propagation direction was not normal to the slip plane. Using aluminum single crystals oriented for single slip, Hikata3 et al. found that during tensile deformation the change of attenuation of the shear wave (actually quasishear) having particle displacements nearly perpendicular to the primary slip direction exhibited the easy-glide phenomena, while longitudinal waves did not. Similar results were reported by Swanson and Green5 during compressive deformation of aluminum crystals. These results are in qualitative agreement with the calculated orientation factors for specimens of this orientation. In well-annealed, undeformed aluminum crystals, the damping is expected to be due to dislocations vibrating on all twelve slip systems. The orientation factors associated with this initial damping will be designated by O2 and O3, where a, represents the average orientation factor for the slow shear (or quasishear) wave and O3 represents the average orientation factor for the fast shear (or quasishear) wave. The calculation of these values for aluminum crystals by Hinton and Green8 shows that they vary very little as a function of crystallographic orientation—at most, by a factor of 2.47. If the dislocation density and loop length are uniform, then in the initial undeformed state, Here the subscript zero refers to the initial value of the attenuation. Also for aluminum, the calculations8 show that the orientation factors for primary slip only, associated with each shear wave, exhibit a sharp minimum for particular crystallographic orientations. A composite plot of the two shear wave orientation factors for primary slip only is shown in Fig. 1. Since these orientation factors are associated with dislocation motion occurring on the primary slip system only, the proper condition to check these factors might be attained by slightly deforming a single crystal oriented for primary slip. For dislocation motion on the primary slip system only,

Jan 1, 1969