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By J. A. Younkins, J. A. Brooke

In 1931 the Philadelphia Company acquired by lease several coal mines in southern Greene County, Pennsylvania. These mines were known as the "Dora," "Seventh Pool" and "Rosedale" mines in the Sewickley seam, and the "Rosemary," "Seventh Pool" and "Warwick" mines in the Pittsburgh seam. All these mines are in the immediate vicinity of Greensboro, Pa., with considerable river frontage on both sides of that village. The mines in each seam are contiguous and to some extent the properties in the two seams lie one above the other. In 1938 the property known as the "Sandy Run mine," in the Sewickley seam, adjoining the Dora mine, was purchased from the Fredericktown Coal and Coke Co. Altogether, by purchase and lease, the company gained control of approximately 3400 acres of coal land in Greene County, from which it was estimated that some 20,000,000 tons of coal could be extracted. Geology of Warwick Properties Both seams of coal outcrop along or near the river on both sides of the town of Greensbgro. They lie on the eastern slope of the Lambert syncline, near the southern end of the axis, consequently the predominant dip of the seams is away from the river, so that development for river handling has the unavoidable disadvantage of adverse grades for haulage to the outside. Predominant grades away from the river at right angles to the "butt" cleat of the coal average about 2.25 per cent dipping in a westerly direction, but local dips occur, which are considerably greater. Predominant grades parallel to the river and at right angles to the "face" cleat of the coal average about one per cent dipping in a northerly direction. Both seams of coal lie in the Monongahela formation, the Pittsburgh bed being the bottom measure of the formation and the Sewickley bed lying about 90 it. above. Approximately midway between the two lies the Redstone coal bed, which is generally thin and of erratic occurrence and therefore of little commercial value. It is mined only locally where it attains sufficient thickness. Sewickley Bed The Sewickley bed is commonly called the "five-foot" or Mapletown" seam, because in Pennsylvania it reaches its greatest thickness and has been mined most extensively in the vicinity of the village of illapletown, approximately one mile west of Greensboro. In the early development of the Warwick properties, which occurred near the river, the seam had an average of 5 it. 2 in. in height. As development proceeded away from the river, however, the height gradually decreased until the average height of the present workings is about 4 ft. 6 in. Present development is encountering lower coal

Jan 1, 1947

By N. S. Stoloff, R. G. Davies

A study has been made of the efject oj different dislocation-precipitate interactions upon the temperature dependence of the flow stress of aged Ni-14 at. pct A1 alloy. It is observed that when the dislocations bow between widely spaced (-20004 coherent Ni3Al particles the flow stress decreases with increasing temperature in the normal way. However, when the dislocations cut closely spaced (-5004 particles the flow stress is independent of temperature from -100 to 600°C, due to a balance between softening of the matrix and an increase in strength of the particles with increasing temperature. The retention of strength at high tempera-tures of commercial nickel-base alloys, which are strengthened by the precipitation of a phase based upon Ni3Al, is thought to be due to the unusual strength properties of Ni3Al. The flow stress of Ni3Al increases continuous1y from -196"C to a maximum at -600"C. It is concluded from a series of thermal-mechanical tests that the sevenfold increase in flow stress over this temperature interval is due to a lattice effect and is not diffusion-controlled. The flow stress of precipitation- or dispersion-hardened materials depends on the resistance to dislocation motion within the matrix and the extra energy required for dislocations to bow between or to cut particles. If the dislocations bow between the particles or if the strength of the cut particles is constant with temperature, then the flow stress of the precipitation-hardened alloy must decrease with increasing temperature due at least to the decrease in elastic modulus of the material. There will be softening also from thermally activated cross-slip or climb, offering an additional degree of freedom for dislocations to avoid particles. For example, in the case of nickel containing a dispersion of thoria,' which most probably deforms by dislocations bowing between particles, the flow stress decreases by about 50 pct between 25" and 650°C. In A1-Cu alloys2 aged to produce the 8" precipitate, dislocations cut the particles, and the flow stress decreases by about 20 pct between -269" and 25°C. However, many commercial high-temperature nickel-base alloys, for example Inconel-X and Udimet-700, exhibit little or no decrease in flow stress with increasing temperature up to about 700°C. A characteristic feature of these alloys is that they are strengthened by the precipitation of a phase based upon Ni3A1. Guard and westbrook4 and flinn' have shown that Ni3Al (and alloys in which a third element such as molybdenum or iron is substituted for part of the aluminum) is unusual in that the hardness and flow stress increase with temperature to a maximum at about 600°C. For the flow stress of a precipitation-hardened alloy to be independent of temperature we propose that the particles must be cut by dislocations moving through the matrix and that the strength of the particle must increase with increasing temperature. Theories of precipitation hardening do not take into account the flow stress of the dispersed particles that are cut during deformation; the only dissipative process usually considered7 is the creation of interface within the particle and between the precipitate and matrix. The purpose of the present investigation has been to study in detail the temperature dependence of the flow stress of a nickel-base alloy strengthened by the precipitation of Ni3Al in two structural conditions such that when deformation occurs it does so by dislocations a) bowing between the particles and b) cutting the particles, respectively. A simple binary Ni-14 at. pct A1 alloy was chosen because considerable information is already available for this system concerning phase equilibria and precipitation reactions and rates.' Dislocation-precipitate interactions in the binary alloy should be similar to those in the more complex commercial alloys. In addition, the mechanical and physical properties of NisAl were studied in detail in the hope of elucidating the mechanism by which the strength increases with increasing temperature up to 600°C. EXPERIMENTAL PROCEDURE For the study of the effect of precipitation of Ni3A1 upon the temperature dependence of the flow stress, an alloy containing 14 at. pct A1 was utilized; a Ni-8 at. pct A1 solid-solution alloy was employed as a comparison material. Vacuum-cast ingots were hot-rolled at 1000°C and cylindrical compression samples, 0.20 in. diam by 0.40 in. high, were prepared from the 1/4-in.-diam rod. Specimens were recrystallized and solution-treated at 1000°C for 1/2 hr and then water-quenched. A preliminary study revealed that, when the Ni-14 at. pct A1 alloy was aged for 1 hr at 700°C, significant precipitation hardening was obtained, and that the structure was free from grain boundary discontinuous precipitation; an overaged condition was produced by annealing the aged specimens at 850°C for 1 hr. To circumvent the difficulties involved in the hot rolling and swaging of Ni3A1, compression samples,

Jan 1, 1965

By M. A. Dayananda, R. E. Grace

Vapor-solid diffusion couples were employed in a study of ternary diffusion in the single-phase copper-rich corner of the Cu-Zn-Mn system Interdiffusion coefficients were measured at three different compositions corresponding to the intersections of diffusion paths determined at 850°C. Intrinsic diffusion coefficients were determined at two compositions by the Philibert-Guy method. New relations between the various intrinsic diffusion coefficients are also presented. MOST of the investigations of ternary diffusion have been made with "sandwich" couples formed by welding together two homogeneous solid solutions with or without markers placed at the interface. With such couples Kirkaldy and his coworkers1,2 have determined interdiffusion coefficients which describe ternary diffusion in the substitutional alloy systems, Cu-Mn-A1 and Zn-Cu-Al. Guy and Leroy3 have reported intrinsic diffusion coefficients for Co-Ni-Cr alloys as a function of composition using the analysis of Philibert and Guy.4 The use of semi-infinite diffusion couples, for example, vapor-solid couples, where the diffusing species are supplied from a vapor source in contact with a diffusion disk, has so far been confined to studies of binary diffusion. Balluffi et a1.5,6 have successfully determined the interdiffusion as well as the intrinsic diffusion coefficients in several binary metallic systems employing vapor-solid couples with markers initially placed at the vapor-solid interface. They have also discussed the general advantages and limitations of such couples. Vapor-solid diffusion couples can successfully be employed in ternary diffusion studies. The importance of such couples in ternary diffusion lies in the fact that inert markers lie close to the vapor-solid interface, and the composition of the marker plane is virtually known before experimentation begins. Another minor advantage is that the method of Philibert and Guy4 may be used with three alloys instead of four. Lastly, the diffusion paths need not be S-shaped, as pointed out by Meijering7 for "sandwich" couples. The Cu-Zn-Mn system is convenient for ternary diffusion studies because of the large single-phase field in the copper-rich corner. The vapor pressure of zinc above such alloys is known, and X-ray measurements indicate that the molar volume is nearly constant over a wide range of compositions.8,9 It is the purpose of this paper a) to extend the analysis of Balluffi and seigle5 to permit an evaluation of interdiffusion coefficients in ternary vapor-solid couples, b) to use the method of Philibert and Guy to determine intrinsic diffusion coefficients with such couples, and c) to present experimental data on both interdiffusion and intrinsic diffusion coefficients for the Cu-Zn-Mn system at 850°C. INTERDIFFUSION IN TERNARY VAPOR-SOLID COUPLES The analysis of Balluffi and seigle5 is extended in this section to a vapor-solid couple where two solutes diffuse from a vapor source into a ternary solid solution. To take into account the expansion of the diffusion disk caused by the absorption of mass from the vapor phase, the total fluxes are expressed on the basis of a coordinate system that moves with the velocity of the vapor-solid interface; thus. where D3ij are the intrinsic diffusion coefficients,4 v(x, t) is the local Kirkendall velocity of mass flow, and F(t) is the negative velocity of the vapor-solid interface (x = 0). Both these velocities are based on a fixed coordinate system far removed from the diffusion zone. Using the continuity relations and Darken's method1' for a ternary system in which components 1 and 2 diffuse from the vapor phase into a solid of negligible vapor pressure, one obtains

Jan 1, 1965

By Lincoln F. Elkins

The Spraberry Trend Field of West Texas was discovered in January, 1949. Drilling of 2.234 wells and production of some 45 million bbl of oil by January, 1953, indicated this to be an important field which will ultimately cover more than 400,000 acres. In addition to being the world's largest field in areal extent, the Spraberry has presented many problems in well completion and operation and has demonstrated unique reservoir performance characteristics. The pay section consists primarily of a few fine grained sandstone or siltstone members in a thousand-ft thick section of shale, limestone. and siltstone. Since porosity averages only 10 per cent and nearly all permeabilities are less than 1 md, conventional core analysis does not delineate the "pay" section. Mercury injection was used as a capillary pressure test adaptable to rapid routine use to select those intervals having low enough connate water saturation to contain commercially significant oil saturation. In the central area of the field this "pay" amounts to 16 ft of Upper Spraberry and 15 ft of Lower Spraberry sands. An interconnected system of vertical fractures, observed in cores, provides the flow channels for oil to drain into the wells hut most of the oil is stored in the matrix since the void volume of fractures is estimated to be less than 1 per cent of that in the sand. Initial potentials of wells range up to 1.000 B/D after fracture treatment which should be compared with estimated capacity of 5 to 10 B/D if oil had to flow into the wells through the sand itself. Without exception initial pressures of later drilled wells were significantly lower than initial pressures of earlier drilled nearby wells in a large area some 6 miles long. This means the earlier drilled wells had drained fluids from areas much greater than their 40-acre proration units. Since most of this performance occurred while the reservoir pressure was above the. saturation pressure it was analyzed by the compressible fluid flow theory. This analysis gave calculated initial presrilres which agreed within 30 psi of measured pressures of 60 per cent of wells in the area using 16-md permeabilitv corresponding to a fracture system substantially that indicated by cores and using combined compressibility of rock and its contained oil and water corresponding to the core analysis data. The most important feature of this analysis was the very close agreement between effective compressibility of the rock and its contained oil and water from the field performance and that from the core tests, because it meant there are no "islands" of low permeability reservoir rock left untapped in the inter-well area and thus no additional wells are necessary to insure that at least one well penetrates each "reservoir." Twenty-five of forty-four 40-acre spaced wells on three contiguous sections were wed in a four-month inteference test. Six shut-in well. were tested monthly for oil production. productivity index. gas-oil ratio and pressure buildup, and seven shut-in wells were tested for decline in reservoir pressure. Tests on 12 regularly producing wells gave comparative data for interpretation of shut-in test wells. Reduction in reservoir pressure, decline in productivity index. and increase in gas-oil ratio were found to be substantially the same in the shut-in test wells as those in the comparative regularly producing wells, meaning that the producing wells were depleting the

Jan 1, 1953

By R. A. Vandermeer, P. Gordon

The study of recrystallization in cold-worked metals is complicated by the impossibility of making direct three-dimensional optical measurements. Metallo-graphically, theinternal three-dimensional features of samples must be inferred from their intersections with the two-dimensional plane of polish. The inherent difficulties involved in this procedure have led— particularly during the last few years—to some instances of rather doubtful interpretations of experimental data in terms of nucleation and growth rates in recrystallization. In the present paper an analysis ; is given of the recrystallization characteristics in a polycrystalline alloy containing 0.008 wt pct copper in ZONE-refined aluminum *and an effort is madf to reemphasize the necessity in such studies for attention to the proper statistical relationships between one- two- and three-dimensional features of opaque samples. It is shown that, in common with several recently described cases for other types of transformations,1-5 recrystallization in this alloy can best be rationalized on the basis that all nucleation took place essentially at time zero—i.e., there is no significant time-dependent nucleation during annealing—and that the kinetics are controlled exclusively by the growth-rate parameters. This is true despite the fact that the number of

Jan 1, 1960

By Richard D. Hagni

Although the ore microscopist routinely examines polished sections to determine the mineralogy and texture of ores, his importance to the solution of problems peripheral to geology is not always fully realized. The techniques which he uses can be applied with little modification to the solution of a wide variety of beneficiation problem. By extending his studies beyond those normally considered to be of interest to the geologist, he can include examinations of polished sections of selected mill products. This is a logical extension, because the minerals and textures in the polished sections of ores are the same as those in millproducts. The mill dressing engineer should be more aware of the types of beneficiation problem that can be solved by the ore microscopist and what the ore microscopist can do for him. A greater degree of cooperation between the ore microscopist and the mill dressing engineer can be of significant mutual benefit. Ore microscopy holds an advantage over chemical analysis, because the interrelations and combinations ofthe mineral constituents of an ore or mill product can be visually determined. This advantage provides solutions to many beneficiation problem. Locking is a type of beneficiation problem that is particularly amenable to ore microscopy. The percentage, type, and distribution of locked particles can be readily determined with the aid of an ore microscope and an estimate made of the extent of additional grinding required for liberation. The extent of intimately locked types, which no reasonable amount of grinding will liberate, can also be evaluated. Mineral coating conditions, free particles of a deleterious mineral, and free particles of a valuable mineral held in flocculated clusters of gangue are other features that can readily be observed. In some instances, visual examination may show that the problem is not one of locking. Photomicrographs illustrate the variety of beneficiation problems for which the ore microscope is applicable. These problems and their resolution demonstrate the importance of the instrument and show the value of close coordination between the mill dressing engineer and the ore microscopist.

Jan 1, 1979

By J. V. Emmons

IT has long been known that the outside skin of tool steel frequently exhibits properties widely different from the interior of the mass. Within the last few years it has been generally recognized that many of these properties were clue to surface decarbonization. The origin and effects of this altering of the composition have been but little studied. C. M. Johnson' arrives at the conclusion that, in annealing, "the most active agent in surface decarbonization is the rust or scale (present on the surface), which is actually reduced to metal at the expense of the carbon in the steel to which it adheres." W. H. Hatfield in his admirable paper, The Chemical Physics Involved in the Decarburization of Iron-Carbon Alloys,' has given us the most tenable theory of the removal of carbon from iron. While Mr. Hatfield's work has been principally clone in connection with the annealing of white cast iron to produce malleable castings, it is frequently applicable to the decarbonization of tool steel. The following equations which he proposed have been fully borne out by the author's experiments: 2Fe3C + 2CO2 = 3Fe2 + 4C0 2C0 + 02 = 2C02 Continuous 2C02 + 2Fe3C = 3Fe2 + 4C0 It is the purpose of the author to show, in a quantitative manner, the effect of various treatments in eliminating the carbon in tool steel. Some of the phenomena of the decarbonized surface will also be described, as well as the practical problems they present to. the manufacturer and user of tool-steel products.

Jan 9, 1914

By R. Norman Orava

The strain-mte behavior of. the tensile yielding and flow characteristics of arc-cast polycrystal-line molyhdenum of pidrity > 99.97 pct was investigated in the range 10-6 to 10-1 sec-1 at 243o, 293o, and 373oK for two grain sizes, 0.027 and 9.098 mm. For 0.998 mm, the strain-mte dependence of the lower yield stress can be described by a straight line of the jowl a, = a + 0 log e over the whole range of strain rates examined. However, for 0.027 mm, the data fit several consecutive linear relationships of the above form. The previous association of these different linear regions with different rate -controlling mechanisms is questionable for molyhdenzdm. The senlilog strain-rate dependence of the yield stress is consistent with Hahn's model for yielding when the stress dependence of the mobile dislocation density, pr, is taken into account. Since p', from rate -cycling experirnents, is found to be relatively insensitive to stress for single crystaIs, the obserzied log-log dependence of their yield stresses is also in agreement with the model. A correction for the stress dependence of p' changes the activation oolurrze for yielding from a zero to a more realislic inverse function of stress where the Peierls mechanism is believed to be rate-controlling. The gmin-size dependence of the lower yield stress is not a monotonic junction of strain rate. RECENT experimental evidence' has revealed that the strain-rate dependence of the tensile lower yield stress, a,, of commercially pure ni- obium and tantalum tested at room temperature can be described by several consecutive semilog relations of the form: sv =a + ß log € [1] where i is the applied strain rate and a and 0 are constant Over only relatively small ranges of strain rate. Three linear regions were found for niobium and four for tantalum. Each linear region was interpreted as being associated with a different rate-controlling mechanism on the basis of the current

Jan 1, 1964

By R. Maddin, C. H. Mathewson, W. R. Hibbard

Recent publicationsl.2 establishing the presence of cross-slip in strained metallic single crystals oriented wholly within the area of single slip as predicted from the generalizations of Taylor and Elam3 described these markings as they appeared during the initial stages of the deformation process. At that time, the plane having a common glide direction with the primary slipping plane was reported as the cross-slip plane although the specific direction was not confirmed. Consequently, in continuation of the research, it seemed advisable to investigate the micro-graphic appearance of cross-slip together with the Laue back-reflection X ray analysis and stress-strain data during the later stages of the deformation process. Accordingly, a single crystal of brass (72.75 pct Cu, 0.01 pct Fe, 0.01 pct Pb, 27.23 pct Zn) was polished mechanically and repolished electrolytically after the manner described in the earlier paper.' Three pairs of flat surfaces, parallel to the specimen axis, and (1) perpendicular to the plane containing the pole of the primary glide plane and the specimen axis, (2) perpendicular to the plane containing the pole of the cross-slip plane and the specimen axis, and (3) perpendicular to the plane containing the slip direction and the specimen axis, were polished mechanically and repolished electrolytically, resulting in a final minimum gauge diameter of 0.4864 in. in a gauge length of 3.36 in. The specimen was elongated in tension and load-extension readings were taken following the method described in the initial investigation.' Observed reorientations were obtained from a series of Laue back-reflection photograms at the center and ends of the gauge length and at various positions around the circumference of the specimen. These were interpreted after the manner of A. B. Greninger.4 Cross-slip (Fig 1 and 2) was found with the first appearance of the primary slip clusters and usually joined members of these clusters. In addition, a third set of entirely different markings (Fig 3) could be noted. The displacement of this third set by the primary slip lines was measured as 8300 at. diam (3.04 microns). Since the specimen was carefully observed at high magnifications before any deformation and no markings of any type could be noted, it would appear that this third set was formed during the deformation process prior to the initiation of classical primary slip. Additional extensions produced no unusual change in the appearance of either cross-slip or the third set of markings. The number of lines increased with increasing elongation and appeared, generally, in areas where earlier markings were present. The continuity of the clusters of cross-slip lines in Fig 4, 5 and 6 illustrates that they are neither noticeably displaced by nor do they displace the primary lines at this stage. In Fig 7, cross-slip appears in a long narrow localized band approximately 45 degrees from the stress axis. This somewhat resembles a twin band except for the lack of a sharp boundary. After a shear of 0.257, suffcient additional glide occurred on the cross-slip plane to displace the primary slip lines (Fig 8). Generally, where a large number of cross-slip lines could be observed in an area on one flat surface, few cross-slip lines appeared on the diametrically opposite position on the parallel flat (Fig 9). These, of course, were not matched observations on the same glide ellipses. It was extremely difficult to make such comparisons. The third set of markings (Fig 10) was extensively displaced by glide on the primary slip planes. A plot of the width of primary slip clusters versus their displacement of the third set of lines is shown in Fig 11. The slope and the linearity of the plot suggest that each primary glide plane slips to a constant maximum value of shear before further slip is transferred to another plane. A shear value of 0.28 was determined in this case. Heidenreich5 has presented a similar schematic representation of glide for aluminum. After the specimen had attained an elongation of 51.8 pct, corresponding to a shear of 0.973, cross-slip appeared very prominently in certain areas as shown in Fig 12, yet at diametrically opposite positions very little cross-slip could be noted, Fig 13. Classical conjugate slip was found at this advanced stage in the deformation, Fig 14, which corresponds to the axial location shown at 12 in Fig 15. It should be noted that cross-slip occurs within the conjugate slip clusters and on the same plane as the cross-slip associated with the closely spaced primary lines which constitute a background in less distinct focus. The third set of markings noted at all stages in the deformation of the

Jan 1, 1950

By L. B. Gittinger

Sulfur is a nonmetallic element widely distributed in nature. It constitutes 0.06% of the earth's crust but only a very small portion occurs in sufficiently concentrated amounts to justify mining. Sulfur occurs in practically all animal and plant life. It constitutes approximately 0.09% of the elements in the oceans; it has been found in meteorites. Sulfur was known and used by man before recorded history. The American Chemical Society approved spelling for the element is sulfur. The English spelling sulphur is used commercially in the United States. In ancient times, sulfur was called brimstone, literally "burning stone." Today the term brimstone is used interchangeably with the term elemental sulfur. Sulfur is found naturally in the elemental form in subsurface deposits associated with gypsum and anhydrite in salt domes and sedimentary formations in evaporite basins and in solfatara-type deposits associated with volcanoes and mineral springs. Sulfur occurs also in molecular combination in ferrous sulfides (pyrites and pyrrhotite) and nonferrous sulfides (copper, lead, zinc, and nickel), and in mineral sulfates (gypsum and anhydrite); as hydrogen sulfide contaminant in natural gas; as organic compounds in crude oil and tar sands; and as pyrite and organic compounds in coal and oil shales. Sulfur resources are abundant and exist throughout the world but the extent to which they can be classified as reserves is greatly circumscribed by prevailing prices and technology. Estimates of world sulfur reserves are compiled by the U.S. Bureau of Mines. A compilation of reserves by area and source of sulfur published in 1970 and presented here as [Table 1] totaled 2.47 billion tons (Lewis, 1970). The effect of the decline in prices which has occurred since the earlier estimate is dramatically illustrated by the 1972 estimate of the U.S. Dept. of the Interior which shows world sulfur reserves of only 1.2 billion tons (Anon., 1972d). Sulfur is produced commercially from one or more sources in nearly 70 countries of the world. World production of sulfur in all forms totaled 41.6 million tons in 1971. (Sulfur statistics given in this chapter are long tons.) Native deposits, sulfides and oil and gas contributed, respectively, 31, 41, and 25% of world production (Table 2). Of the sulfur produced from native deposits, salt domes accounted for 54% and evaporite basin deposits, 44%. Volcanic deposits are of little significance except for local consumption. The past two decades have seen important shifts in the world's sulfur sources. In 1950, native deposits and sulfides each supplied about one-half of the world's production. During the 1950s, sulfur recovered from oil and natural gas grew rapidly, representing about 10% of the total by 1960. Since then, the petroleum industry has continued to increase its relative importance as a source of sulfur, representing more than 30% at 1972 year-end. Sulfur is generally classified as elemental or nonelemental for statistical purposes. Elemental sulfur is sulfur produced in the pure, uncombined form. It includes production from native deposits, as well as that recovered in the elemental form from oil and natural gas or other sulfur-bearing materials. When produced from other than native deposits, it is generally referred to as recovered elemental sulfur. Nonelemental sulfur is that which is utilized commercially in molecular combination with other elements, such as sulfides or sulfates. Elemental sulfur is being produced from salt dome deposits in the Gulf Coast region of the United States and the Isthmus of Tehuantepec in Mexico, and from evaporite basin deposits in west Texas, Poland, Sicily,

Jan 1, 1975

By J. P. Matoney, E. J. Sandy, D. A. Dahlstorm

INTRODUCTION Before an understandable discussion concerning coal-dewatering processes can be initiated, it is necessary to define some terms of usage. The many different meanings and interpretations of terms preclude development of standard definitions so that the terms which are defined in this chapter should be regarded mainly as working terms intended to facilitate communication. A coal slurry ' might be defined as a watery suspension carrying particles of fine coal and other assorted material ranging upward in size from the finest clay particles. Some particles may be in the colloidal sue range and exhibit characteristics of suspended colloids. The dilution of the system generally is such that it is in a condition of independent particle subsidence. In some coal mining areas a slurry is regarded as a suspension of fine coal and other materials having a dilution that cannot be economically dewatered by filtration. A coal slime may be regarded as a slurry containing particles of such size range that 50 per cent or more (by weight) will pass a 200-mesh sieve. Slime suspensions generally are difficult to handle without special treatment in conventional sedimentation equipment. A coal sludge is defined as a slurry that has been partly dewatered by sedimentation usually to a thick or viscous consistency where further dewatering can be most readily facilitated by filtration. Culm and silt are terms characteristic of coal-preparation practice which should be defined. In anthracite terminology, culm is the generally coarse residue or waste accumulation of coal, bone and rock from preparation plants most of which are no longer functional. Culm has a wide range of sizes, some rather coarse, and except to differentiate it from silt, the term is of limited interest in this discussion. In anthracite terminology, silt is the accumulation of waste fine coal, bone and slate settled out from preparation plant water in excavated basins. Silt is generally made up of particles ranging in size from 3/32-in. round-opening screen to the very finest sues. Silt is also referred to at times as sludge, fines, slush, and mud and is the partly dewatered derivative of what has been previously defined as slurry. In the terminology of the bituminous coal producing areas, the word culm commonly corresponds to slurry or slime, depending upon the size distribution of the suspended solids. Editor's Note: Because of the numerous and varied contributions of the associate authors of this chapter, the text does not differentiate between sections authored by each individual as is the case in most chapters of this book.

Jan 1, 1968

By Sidney A. Swensrud

MUCH discussion has occurred as to the use or uses which might be made after the war of either or both .of the large diameter (24 inch and 20 inch) War Emergency pipe lines built by y the United States Government during the war, to move crude petroleum and refined products such as gasoline and light distillate fuels. Indeed, the disposition and future use of these lines constitutes, in the minds of many people, one of the most important problems of postwar readjustment in the Oil Industry. The two lines, running from points in Texas to the New York-New Jersey-Philadelphia area, were constructed only because of the inability during the war to continue normal ocean tanker movements from the Gulf Coast to the East Coast. Physically they could continue after the war to move crude or refined products, and it appears that lines of such large diameter as these, if operated at or near capacity, could move these liquids at costs per barrel which might be considered in the same general cost range as for tanker movements.1 If, therefore, we were to look forward at the end of the war to a shortage of tankers, it is probable that the continued use of these pipe lines for petroleum movements to the East Coast would be worth considering, as against building new tankers to take over the movement, provided there were no other economic or national defense reasons for restoring tanker fleets and no other better use for the pipe lines. Because of the extensive tanker construction program which has been and still is in progress, and because of our Navy's marked success in combating the submarine problem, it appears to be quite possible, however, that instead of a shortage of tankers at the end of the war, we may have a surplus instead. If this should turn out to be the case, then there would seem to be considerable doubt that these lines would continue to be used for moving petroleum or products to the East Coast at the expense of tying up tankers. It would hardly seem probable that the owner of any such tankers would ship via one of the large lines at the expense of tying up one of its own tankers, unless the pipe line tariff rate charged was lower than the out-of-pocket cost of operating a tanker as against the out-of-pocket cost of keeping it tied up. And considering that a substantial part of the cost of operating a tanker goes on even when it is tied up, it is very difficult to figure out how any pipeline tariff could be established that would be low enough to compete with individually owned tankers that otherwise would be idle. Certainly a pipe line tariff rate high enough to cover direct costs plus even a low rate of depreciation and return on the investment would be far above the out-of-pocket tanker operating costs. In view of these considerations, it has seemed desirable to examine with some care some of the various alternatives that have been suggested as to other possible uses to which these lines might be put. One of these is for transportation of natural gas to the New York-New Jersey Philadelphia area. This Eastern area, located at the destination of these lines, contains the heaviest concentration of population in the United States, and is not now served with natural gas. At the other end of the lines lie the greatest discovered natural gas reserves in the United States, if not in the world, and many

Jan 1, 1944

By T. E. Leontis

Data are presented in this paper to show that addition of zirconium to sand-cast Mg-Th alloys effects a marked decrease in the grain size of these alloys which is accompanied by a significant increase in the mechanical properties over the entire range of thorium content investigated. The beneficial effect of zirconium on the strength properties is maintained at elevated temperatures up to 700°F. In addition the alloys exhibit exceptionally high creep resistance at temperatures up to 600°F. Zirconium does not greatly improve the strength or creep characteristics of extruded Mg-'Th alloys. Cerium is not a desirable addition to Mg-Th-Zr alloys. IN a previous paper,' it was shown that addition of thorium to magnesium imparts exceptionally high resistance to creep at elevated temperatures both in the sand-cast and in the extruded states. The large grain size of the sand-cast alloys, however, renders them of questionable value as engineering materials. Sauerwald² showed that the grain size can be reduced effectively by the addition of zirconium. Results of a detailed study of the properties of Mg-Th-Zr alloys over a wide range of thorium content are presented in this paper. In accordance with the preliminary findings of Sauerwald,² it is shown here that Mg-Th-Zr alloys possess the unusual combination of fine grain size and a high level of strength and creep resistance at elevated temperatures. Some information on the effect of cerium on the properties of Mg-Th-Zr alloys is presented also. Effect of Th on Solubility of Zr in Molten Mg Sand-cast test bars and 3 in. diam extrusion billets of Mg-Th-Zr and Mg-Th-Ce-Zr alloys* were pre- pared according to the procedures described in the previous paper.' The zirconium was added in the form of sponge metal as supplied by the Bureau of Mines.' The maximum amount of zirconium that usually can be introduced into magnesium at the customary alloying temperature of 1350° F is about 0.7 pct. The analyses in Table I clearly show that thorium in- creases the solubility of zirconium in liquid magnesium. The tabulated zirconium contents are designated as "acid soluble;" this serves to distinguish these values from the small amount of zirconium that is not dissolved when the alloy is subjected to the action of a dilute acid solution. The "acid-insoluble" zirconium is believed to be ineffective as an alloying ingredient. The acid-insoluble zirconium contents ranged between 0.03 and 0.16 pct in the present alloys, the tendency was toward higher values in alloys with higher thorium content. In contrast to the effect of thorium, cerium decreases the solubility of zirconium in magnesium. This is shown by the three Mg-Th-Ce-Zr alloyst in- cluded in Table I and stands in agreement with the observations of Nelson and Stricter".' on Mg-misch-metal-Zr alloys. Effect of Zr on Grain Size of Mg-Th Alloys The potent effect of zirconium as a grain refiner has been demonstrated for many types of magnesium alloys.3-8 Of greatest importance to date are Mg-Zn-Zr alloys5,6,8 and Mg-mischmetal-Zr alloys.3,4,7 Zirconium has also been found to exert a marked grain-refining action on Mg-Th alloys. All the Mg-Th-Zr alloys cast in the form of ½ in. diam test bars have an exceedingly fine grain size (Table I). Reference to the previous paper' will show that binary Mg-Th alloys containing up to 6 pct Th are almost completely columnar even in the M in. diam reduced section of a test bar, and that 10 to 50 pct Th alloys have an equiaxed grain structure of 0.03 to 0.08 in. The data in Table I also show that addition of cerium to Mg-Th-Zr alloys has no effect on the grain size. In addition to increasing the strength properties, the fine grain size of Mg-Th-Zr alloys

Jan 1, 1953

By Anton Sawatzky, Erich Vogt

By means of mathematical solutions to the appropriate diffusion equations, we describe the kinetics of the thermal diffusion of hydrogen in Zircaloy-2 for the various temperatures and concentrations encountered in a heavy water moderated reactor. When the hydrogen concentration is below terminal solid solubility only the a Phase is present. Redistributions are then described in terms of the characteristic functions of the difhsion equation. For higher concentrations both the a and 6 phases are present. We assume the two phases to be always in equilibrium. For moderately small hydrogen concentrations exact solutions of the two-phase equation approach the the approximate solutions derived by Sawatzky and for all concentrations the exact solutions exhibit the qualitative features of his result: the two-phase concentration increases with time, everywhere; in the absence of a hydrogen current at the hot end of the sample an a-phase region always exists there; the interface of the a + 6 , a-phase boundary moves toward the cold md of the sample and the hydrogen concentration is discontinuous at the interface. Simultaneous solulions of the a and a + 6 hydrogen distributims and of the concomitant interface motion are obtained and compared to the observations of Sawatzky and Markowitz. The kinetics of the hydrogen diffusion process are shown to lead to m apparent heat of transport of the a phase which is lower than the actual value (even for samples with long anneals) thus resolving at least partially the disparity between experimental measurements of this quantity. A number of recent papers1"4 have reported measurements on the diffusion and redistribution of hydrogen in Zircaloy-2 under temperature and concentration gradients. These studies were instigated by problems arising from increasing use of Zircaloy-2 as a fuel element cladding material in pressurized-water power-reactors. The Zircaloy-2 picks up hydrogen during the operation of the reactor: the consequent precipitation of zirconium hydride in the Zircaloy-2 has pronounced effects on its mechanical properties. The Purpose of the present Paper is to describe the kinetics of the thermal diffusion of hydrogen in Zircaloy-2 for the various hydrogen concentrations and temperatures likely to be encountered in reactors. When the hydrogen in the Zircaloy-2 is entirely in the solid solution phase (a phase), the differential equation for thermal diffusion is well known and the redistribution can be described by standard mathematical methods some of which are given in Section 11 below. The treatment of the a + 6 (hydride) region differs from the earlier treatment of sawatzky3 by taking into account several modifications of the two-phase diffusion equations as suggested to us by Markowitz4 and Kidson.5 Even with the modifications the results obtained in our more complete treatment are substantially the same as those found by Sawatzky. As we show, the difference between the results of sawatzky3 and kIarkowitz4 is largely due to the difference in the geometry of their experiments. In the next section we derive the modified two-phase equation for arbitrary geometry. The exact solution of this equation is given in Section III for linear and cylindrical geometry. It is shown that Sawatzky's approximate solution is quite accurate for almost all the temperatures and hydrogen concentrations which are actually encountered. In Sawatzky's approximate theory the hydrogen concentration everywhere in the two-phase region increases continuously. As his paper pointed out, this result, together with hydrogen conservation, implies that in a sample with no hydrogen current flowing into the hot end a two-phase region is always accompanied by a single-phase region at the hot end of the sample. The net hydrogen gain in the two-phase region is supplied by the decrease of hydrogen in the single-phase region and by the movement of the (a, a + 6) boundary toward the cold end of the sample. Hydrogen conservation at the (a, a + 6) boundary leads to a discontinuity in the concentration and its derivative there. In Section IV it is shown how these qualitative features of the thermal diffusion kinetics arise from the simultaneous solution of the a-phase differential equation and a + 6 phase equation. Methods derived by us previously for the solution of the redistribution in both phases and the accompanying motion of the boundary are used to obtain approximate solutions valid for large times. The solutions account well for the observed redistributions of Sawatzky and Markowitz. It is shown how the continuing motion of the (a, a + 6) boundary leads to measured values of the heat of transport lower than the actual value, even for specimens with relatively long anneals.

Jan 1, 1963

By H. T. Shore, J. M. Schultz

A number of experimental rnethods—X-ray powder diffractometry, Laue photography, X-ray small-angle scattering, and transmission electron microscopy and dijfraction—have been utilized to examine the morphology associated with precipitation from the terminal, g, solid solution of a Zn-1 pct Cu alloy. A significant age hardening was observed in a 1 pct Cu alloy. X-ray and electron diffraction results showed that the structural inhomogeneities associated with the hardening were isotructural with the matrix. The average size and shape of the inhomogeneities were deduced from the electron microscopy and X-ray small-angle scattering. The preprecipitates are hexagonal platelets some 300? in diam. and some twelve unit cells thick. The orientation of the platelets was deduced from Laue photographs and electron diffraction. The platelet plane is (0001). When a large amount of pre-precipitation is present in a localized volume the new lattice is often disoriented by a rotation about (0001) of of the matrix. WhILE dilute Zn-Cu alloys have been commercially important for some 50 years, relatively very little is known metallographically about this material. The "Zilloys", zinc with about 1 wt pct Cu and sometimes a small addition of magnesium, are used to produce rolled zinc which is harder and stronger than that produced by other rollable zinc alloys.' According to the phase diagrams of the zinc-rich side of the Cu-Zn system, such dilute Zn-Cu alloys should age-harden;2-5 the solubility of copper in zinc, g-phase, at 424°C is 2.68 pct, while at 0°C it is only to 0.3 pct. However, the published literature on the aging of this system appears to be limited to a documentation of the contraction of 1, 2, and 3 pct Cu alloys aging at 95°c,6 and an attempt to measure changes in lattice parameters during aging.' In the latter work, no lattice parameter changes were detected, although a broadening of the highest-angle lines was detected and considerable diffuse scattering was observed. Micro-structural investigations have been limited to the latest stage of aging, wherein Widmanstatten precipitates are formed.3,47 These alloys are of interest for still another reason. The two most zinc-rich phases in the Cu-Zn system, 77 and E, are both hcp. Moreover, the change in a, between 17 and t for a 1 wt pct Cu alloy is onlv 3.64 -,~ct: the change in Co is 12.0 ict. It would be anticipated that precipitation in such a material might occur through metastable phases or G.P. zones with epitaxy along mutual 0001 planes. The goals of the present work are aimed at partially filling the void of knowledge concerning the early stages of precipitation from the g phase. In particular, we have attempted to document the magnitude of the age hardening of this system and to determine the size, shape, and orientation within the matrix of the elements of precipitation in an early stage of condensation. EXPERIMENTAL A) Specimen Preparation. Specimens were prepared In two somewhat different ways, one method being used for X-ray Laue and diffractometer measurements, optical microscopy, and Rockwell hardness measurements and the other used for electron microscopy and X-ray small-angle scattering. In the first case zinc and copper in the proper proportions to yield a 1 wt pct Cu alloy were melted together in a closed graphite crucible. Castings so made were free of apparent segregation or oxidation. The castings were then solution-annealed at 400°C for several days and then quenched in water to room temperature. Filings of portions of the specimens were made for use as X-ray powder diffractometry specimens. The electron microscope material was made as follows. Castings were made under vacuum with copper powder placed inside a hollow zinc cylinder to insure good contact of the materials. These 1 wt pct Cu pieces were then rolled to 0.1 mm with an intermediate anneal in vacuo. The rolled sheets so formed were then annealed for about 6 hr at 225°C. Finally the specimens were electropolished slowly until thin enough for transmission electron microscopy. The polishing is discussed in greater detail in the Results section. B) Measurements. X-ray measurements of three types were performed. A G.E. XRD-5 diffractometer was used to examine powders of the alloy for identification of second-phase material. A Kratky small-angle camera, also operating from a G.E. tube, was used to investigate the sizes of small precipitate particles. In both cases, nickel-filtered copper radiation was utilized. Finally, individual grains of the large-grained castings were examined in the back-reflection Laue geometry. Electron microscope studies were carried out with a J.E.O.L. Model 6A instrument. RESULTS A) Hardness Measurements. Hardness measurements performed at room temperature on the large-grained polycrystalline specimens showed a hardening which was essentially complete in 3 hr. Fig. 1 shows a typical plot of hardness vs aging time. The relative magnitude of the ultimate hardening varied from run to run between 150 and 200 pct of the value for the material immediately after quenching from the solution anneal. Most probably the variations reflect small changes in the time taken to remove the specimen from the vacuum furnace after the solution anneal.

Jan 1, 1969

By H. H. Podgurski, H. E. Knechtel

Annealed Fe-Al alloys do not react readily to form AlN when held at 500ºC in NH3-H2 gas mixtures, but do so upon the introduction of dislocatims. Nuclea-tion of the nitride phase occurs on dislocation sites. In turn, the growth of the aluminum nitride particles causes the ferrite phase to yield plastically, generating more dislocations for the nucleation process. The nitride phase extracted from an Fe-2 pct A1 alloy nitrogenated at 500°C was identified as stoichio-metric aluminum nitride with a hexagonal crystal lattice. THIS investigation reveals the role that dislocations play in initiating and sustaining the nitriding reaction in Fe-A1 alloys. As early as 1931 the work of Meyer and Hobrock1 suggested that the initiation of the nitriding reaction could involve a nucleation controlled process. Recently Bohnenka2 depicted the gas-phase nitriding process below 600°C as one of mixed control limited by nitrogen penetration through the surface, by nitrogen diffusion, by aluminum diffusion, and by nucleation of the nitride phase, Fig. l(a). In our research in a comparable alloy (0.57 pct Al) at 575ºC, we have observed a nitrogenation which we feel is better described by Fig. l(b). In the case of a 2 pct-A1 alloy partially nitrided at 500°C we propose the profiles shown in Fig. l(c). For a complete and accurate description of the process, a concentration profile of the dislocation density in the test specimen would be needed. EXPERIMENTAL Nitrogenization was conducted between 500" and 575°C in a variety of NH3-H2 gas mixtures on three Fe-A1 alloys: 1) zone-refined iron + 0.16 i 0.2 pct Al—levita-tion melt, 2) zone-refined iron + 0.57 0.02 pct Al— levitation melt, 3) plastiron + 2 pct Al—melted by induction heating. To demonstrate the effect of dislocations on reactivity, both cold-worked and annealed samples were investigated. All nitrogenation rate studies were conducted gravimetrically with a gold-plated invar balance4 contained in a gas-flow system. To avoid contamination of the specimens in the reaction zone of the system, the reaction chamber was constructed of high-purity dense alumina. The activity of nitrogen was fixed by specific NH3-H2 gas mixtures whose compositions were continually monitored by calibrated thermal conductivity gages and checked by chemical analysis. Variations of ± 0.1 pct NH3 could easily be detected by both methods. Throughout this paper the activity of nitrogen is defined as PN3 /PH23/2 , where PNH3, and Ph2 are partial pressures in atmospheres. Electron transmission, density measurements, and chemical analyses were made on specimens before and after nitrogenating in order to reveal structural and chemical changes. Similar studies as well as X-ray diffraction studies were conducted on nitride extractions from the nitrogenated 2 pct-A1 alloy. These extractions were obtained by the use of an anhydrous bromine-methyl acetate solution which dissolves the iron and leaves the insoluble nitrides as a residue. Hardness profiles were obtained on cross-sections of partially nitrided specimens to demonstrate the extent of nitriding through the thickness of the specimens. RESULTS AND DISCUSSION The nitrogen activity in the NH3-H2, atmospheres was never allowed to reach a level capable of producing iron nitride (Fe4N). Hence, the term nitriding as used in this paper refers only to the formation of aluminum nitride whereas nitrogenation refers to the total uptake of nitrogen regardless of how it is distributed throughout the alloy. The weight increases observed during the initial stage of a nitrogenating treatment are due primarily to the solution of nitrogen in the ferrite phase, particularly when starting with annealed specimens. Because this initial nitrogenation rate in the case of the 0.57 pct A1 alloy, see Figs. 2 and 3(a), was most rapid the weight change that occurred thereafter might be attributed to the nitriding reaction with the exception of a small weight increment due to the irreversible pickup of oxygen by aluminum. The oxygen (<70 ppm) came from traces of H2O and 0, in the hydrogen and ammonia gases. On the basis of discrepancies between total weight increase and the increase in the nitrogen content of the sample as determined by chemical analysis, it was estimated and later established by activation analysis, that as much as 200 ppm of oxygen were taken up by a fully nitrided Fe-0.57 pct A1 specimen at 575°C. Most of the oxygen could have been picked up from the nitriding atmosphere on the surface of the samples during cooling to room temperature. Even 50 ppm of water in the gas phase will become oxidizing to iron before the sample has cooled to room temperature. The lack of reactivity* of these alloys in the annealed

Jan 1, 1970

By D. Walton, B. Chalmers

A preferred orientation is known to occur frequently in the columnar zone of castings. This has been attributed to a preferred direction of growth. However, no satisfactory mechanism was proposed by which the preferred direction of growth led to the preferred orientation. The purpose of this work has been to establish this mechanism. It has been found that in general the observed preferred orientations only develop when the preferred directions of growth reveal themselves by dendritic growth. A mechanism based on this premise is found to be in agreement with the experimental data obtained in the course of this work. WHEN a liquid metal is allowed to solidify in a mold, it usually freezes in three stages, distinguished from each other by the size and shape of the grains. The first zone to freeze (the chill zone near the mold wall) consists of relatively fine grains that are equiaxed in shape and random in orientation. The next zone consists of crystals that are elongated in the direction of heat flow, i.e., normal to mold wall. These crystals are much larger in cross section than the crystals of the chill zone and have a very strongly preferred orientation. This is the columnar zone. The final zone, which is absent in very pure metals, is again equiaxed and randomly oriented, but usually has a much coarser grain size than the chill zone. The purpose of this study is to describe and account for the crystal size and orientation in the columnar zone. The occurrence of a preferred orientation in the columnar zone is well known, and in 1940, Greninger&apos; suggested that it is apparently related to dendritic growth although at that time the only data were for metals with the face-centered-cubic structure. Table I shows that the direction of dendritic growth and the crystal axis that follows the heat flow direction coincide in all cases so far studied. The term "dendritic growth" is used here to represent the branched type of morphology that is characteristic of growth into supercooled melts.&apos; In addition to the supercooling which is necessary before nucleation will occur at the mold wall, the necessary supercooling for continued dendritic growth can be provided in a mold by heat flow into the already formed solid at an interface whose Liquidus temperature is depressed by an accumula-

Jan 1, 1960

By J. A. Younkins, J. A. Brooke

In 1931 the Philadelphia Company acquired by lease several coal mines in southern Greene County, Pennsylvania. These mines were known as the "Dora," "Seventh Pool" and "Rosedale" mines in the Sewickley seam, and the "Rosemary," "Seventh Pool" and "Warwick" mines in the Pittsburgh seam. All these mines are in the immediate vicinity of Greensboro, Pa., with considerable river frontage on both sides of that village. The mines in each seam are contiguous and to some extent the properties in the two seams lie one above the other. In 1938 the property known as the "Sandy Run mine," in the Sewickley seam, adjoining the Dora mine, was purchased from the Fredericktown Coal and Coke Co. Altogether, by purchase and lease, the company gained control of approximately 3400 acres of coal land in Greene County, from which it was estimated that some 20,000,000 tons of coal could be extracted. Geology of Warwick Properties Both seams of coal outcrop along or near the river on both sides of the town of Greensbgro. They lie on the eastern slope of the Lambert syncline, near the southern end of the axis, consequently the predominant dip of the seams is away from the river, so that development for river handling has the unavoidable disadvantage of adverse grades for haulage to the outside. Predominant grades away from the river at right angles to the "butt" cleat of the coal average about 2.25 per cent dipping in a westerly direction, but local dips occur, which are considerably greater. Predominant grades parallel to the river and at right angles to the "face" cleat of the coal average about one per cent dipping in a northerly direction. Both seams of coal lie in the Monongahela formation, the Pittsburgh bed being the bottom measure of the formation and the Sewickley bed lying about 90 it. above. Approximately midway between the two lies the Redstone coal bed, which is generally thin and of erratic occurrence and therefore of little commercial value. It is mined only locally where it attains sufficient thickness. Sewickley Bed The Sewickley bed is commonly called the "five-foot" or Mapletown" seam, because in Pennsylvania it reaches its greatest thickness and has been mined most extensively in the vicinity of the village of illapletown, approximately one mile west of Greensboro. In the early development of the Warwick properties, which occurred near the river, the seam had an average of 5 it. 2 in. in height. As development proceeded away from the river, however, the height gradually decreased until the average height of the present workings is about 4 ft. 6 in. Present development is encountering lower coal

Jan 1, 1947

By Frank J. Tolonen, Nicholas H. Manderfield, Paul Jasberg

EARLY in the study of the low grade iron formations of Michigan, wide variations in their structure and texture became evident. Because of these variations no simple method of concentration is possible, and those portions of the formations that can be exploited profitably under a given stage of metallurgical progress and existing economic conditions must be searched for carefully. Both structure and texture of the formations have an important bearing on their amenability to bene-ficiation. By structure is meant the banding planes of easy fracture, the porosity, and the degree of leaching. Texture, which includes grain sizes, shapes, and degree of interlocking, determines the amount of grinding necessary to liberate the mineral grains. Structure determines the liberation of portions richer in one mineral. Structure and texture may be termed the gross features of the formation. Earliest surveys of the formations were conducted to outline the parts that could be concentrated at % in. (3 mesh). Operators agreed on this size because anything finer required sintering or other agglomeration processes. At 3 mesh only the structural features, as defined above, would be liberated. With suitable ores concentration was easy, as any of the gravity methods could be used. Sink-and-float gave good results, but with this method only limited portions of the iron formations yielded a desilrable product.1,2 n general, the iroa content could be raised to shipping grade, but the silica content remained too high—sometimes 20 pct—instead of 9 or 10 pct. Grinding did not greatly increase the liberation ofsilica until 2010 mesh or finer was reached. To find the reason fpr this T. M. Broderick began micros~opic examin&apos;ations of the formations in 1933.3 Procedure: The purpose of this discussion is to correlate the appearance of typical portions of the iron formations with their amenability to concentration. As liberation is essential before separation becomes possible, much of the work is based on measuring the liberation achieved by crushing and grinding. Both heavy media and magnetic tube tests were used in this work. On the basis of general structural features such as banding, degree of alteration, and leaching, a specimen was selected from each part of the iron formations studied. The specimen represents the gross features of the formation and not necessarily the particular formation quantitatively. One half of the specimen was polished for macro-study, and the remainder was used for analyses to obtain the grades represented by variations appearing in the macrosection. Specimens for microscopic examination were also prepared for each variation in gross appearance. For correlation of microstructure with liberation, the previous work by sink-and-float methods was supplemented by magnetizing roasting followed by magnetic separation. The results show the liberation of silica to be very important at the sizes used, because any silica particle with iron minerals occluded would be held in the concentrate. A magnetizing roast changes the crushing and grinding character of the sample. For partly leached soft samples the change is slight, but with harder types and those in which there is a considerable change in crystal structure of the minerals, the increase in liberation of the iron minerals may be 30 pct more than that of unroasted samples at the same crusheH size. Gogebic Range Iron Formations: The Gogebic Iron Range is located in the extreme western and southern parts of Michigan&apos;s Upper Peninsula, extending westward into Wisconsin. Samples for this study were obtained from the Ironwood formation, comprising three chief members—the Plymouth, Norrie, and Ahvil—with several intermediate slates and thick overlying slates. (The slates are not considered in this discussion because grinding finer than present practice is usually required to liberate the iron minerals.) The predominant iron mineral is hematite, about half of which is hydrated to goe-thite. Limonite occurs in some of the partly leached areas, and siderite in parts of the formation.

Jan 1, 1958

By Richard H. Hopkins, R. W. Kraft

A new technique facilitating the rapid determination of the three-dimensional morphology of phases suspended in an opaque matrix is described. The vapidity of the technique is based upon continuous cinephotomicrographic recording of specimen microstructure as the specimen surface is removed under controlled conditions in an electrolytic cell. The advantages of the technique for determining spatial morphologies in opaque materials are illustrated by application of this method to the study of the configuration of faults in a specimen of directionally solidified CuAl2-Al eutectic alloy. A spatial model of the eutectic fault network deduced in this manner has substantiated the facts that faults in this alloy tend to lie parallel to one another in a direction close to that of the specimen growth axis and that the majority of faults tend to bridge lamellae rather than run parallel to them as growth proceeds. For the specimen studied fault density decreased as growth proceeded. ALTHOUGH metallographic observation is a powerful tool for investigating the correlation between structure and properties in metallic alloys, ordinary metallographic methods suffer the fundamental limitation that any conclusions concerning the three-dimensional structure of these opaque materials must rely upon inference from two-dimensional microsections. For this reason it is frequently impossible to make valid judgments regarding the true spatial distribution of the micro-constituents in specimens under investigation. Several techniques have been devised to circumvent the basic limitation of planar microsec-tioning and employed with varying success. These include construction of three-dimensional models of alloy microstructure from sequences of photomicrographs,1-3 quantitative deduction of spatial features based upon statistical studies of data from random and/or selected plane microsections,4-6 and selective dissolution of one phase in a two-phase alloy to reveal the topography of the phase remaining.&apos; However these techniques also have certain obvious disadvantages. Construction of three-dimensional models is a very time-con- suming procedure due to the tedious polish-etch-photograph cycle needed to obtain the necessary photomicrographs to portray the spatial microstructure. Statistical methods by their very nature give only average values of the quantities being studied and cannot therefore give a detailed physical picture of the microstructure to be observed. Finally, the technique of selective dissolution is only applicable in systems where the phases are of vastly different chemical reactivity; it is of little use in the study of single-phase alloys. Since the determination of the three-dimensional structure of opaque materials is hindered by two facts—the materials are opaque to radiation in the visible spectrum and construction of spatial models of microstructure is quite laborious—two solutions to the problem suggest themselves: 1) use radiation of energy great enough to render the alloy transparent, i.e., some microradio-graphic method, or, 2) devise a rapid means to section and record alloy microstructure. Stereomicroradiography has indeed been used to study internal arrangements of phases in several materials8,9 but the method, in general, is limited to very thin specimens (due to X-ray absorption) and simple microstructures. It would seem then that development of a rapid, simple, and generally applicable technique for studying the details of alloy microstructures in three dimensions can best be undertaken by following the second approach above. Using this idea a new technique for rapid evaluation of spatial microstructures was developed based upon cinephotomicrographic recording of the micro-structure of a specimen undergoing controlled electrolytic dissolution. It was further felt that application of this technique to the careful study of the spatial configuration of faults in a CuAl2-Al eutectic alloy would yield information that could be correlated with the extensive data3,6,10-12 already compiled concerning the solidification and crystallography of this eutectic. The practicality and usefulness of similar methods for studying three-dimensional features in alloys has recently been illustrated by the study of dislocation loops in zinc13 and spheroidized structure in steel.14

Jan 1, 1965