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By G. Krauss, W. Pitsch

The fine structure of the bcc martensite formed in an Fe-33 wt pct ATi single crystal of arrstenite is sho~on by transmission electron microscoPy to consist of combinations of transformation twins, stacking faults, deformation twins, and regular arrays of parallel screw dislocations. These structures constitute evidence for the multiple lattice-invariant deformations which operating during the formation of martensite could produce the real habit-plane scatter measured by a two-surface analysis of the plates formed in the single crystal of this investigation and reported in the literature for other Fe-Ni rnartensites. CRYSTALLOGRAPHIC theories1,2 of martensitic transformation show that the habit plane of martensite in a parent lattice is dependent in part upon an inhomogeneous distortion or lattice-invariant deformation which takes place on a fine scale within a martensite plate during its formation. Several recent theoretical papers3,4 have addressed themselves to an analysis of a wide variety of conceivable lat-tice-invarient deformations and the habit planes which they produce, while experimental investigation have been concerned with either the measurement of habit planes or the description and identification of the martensitic fine structure which reflects the nature of the lattice-invariant deformation operating during transformation. In Fe-Ni alloys with subzero Ms temperatures, the group of alloys with which this paper concerns itself, habit planes have often been found to scatter an amount greater than might be expected from possible experimental errors,5-7 and fine twinning has been identified as a major constituent of the fine structure of martensite.8-11 It has been suggested3,4 that more than one type of invariant shear occurs during martensitic transformation. This possibility has been experimentally supported12,13 by the observation of both dislocation configurations and twinning in a single martensite plate. The purpose of this paper is to report additional evidence for multiple lattice-invariant deformations in martensite and so to account for the real scatter in the habit planes of the martensite plates formed in Fe-Ni alloys. EXPERIMENTAL PROCEDURE The Fe-Ni single crystal was produced by pulling a high-purity iron and nickel charge through a single-crystal vacuum furnace in an alumina crucible. The crystal was double-melted to promote homogeneity and to increase its size by further additions on the second pass. In its final form the crystal was 4 cm in diam and 5 cm long. The nickel and carbon contents were analyzed at 32.9 and 0.006 wt pct, respectively. The austenite of this alloy first transformed to martensite by bursts at about -120°C, and, to preserve as much of the austenite as possible, all transformation was performed just below -120°C. Some observations were made on transformed samples which had been heated for 2 min at 340°C. It is assumed that the features of the martensite of these samples, Figs. 1 and 4, are the same as those of the as-quenched martensite. Orientation of the crystal by X-ray diffraction established 10.735 0.609 0.3161? as the axis of the crystal, an orientation that was checked within 2 deg by neutron diffraction. Further checks by electron diffraction of samples cut normal to the axis confirmed this orientation within the larger limits of error inherent in electron diffraction of thin foils. The X-ray orientation was the one used for the two-surface analysis of the martensite habit planes. A two-surface analysis was performed on the quadrant of the single crystal which had been oriented by both X-ray and neutron-diffraction techniques. Photomicrographs at X50 were made on two surfaces along an edge 2 cm long. Fiducial marks and the fact that many of the plates were almost completely surrounded by retained austenite made good matching of individual plates on two surfaces possible. The habit-plane trace on a surface was taken as the best line parallel to the long axis of a plate. A measure of the accuracy afforded by this criterion was provided by a family of very large plates which appeared at intervals along the entire 2 cm length of the edge. The plates all had habit-plane traces within 2 deg of one another. Many of the plates did not show midribs and, therefore, the use of midribs7 to represent habit-plane traces was not feasible in this investigation. The over-all experimental accuracy is estimated to be better than ±2 deg. Samples for transmission examination in a Siemens Elmiskop I at 100 kv were prepared by cutting 2-mm-thick discs from the single crystal, removing about 0.5 mm by chemical polishing,14 trans-

Jan 1, 1965

By J. Brett, L. Seigle, L. Castleman, T. Montelbano

Impurity-induced low-temperature recrystallization of cold-worked tungsten was inuestigated with emphasis on the influence of nickel on the reaction. Palladium, nickel, aluminum, manganese, platinum, and iron greatly lower the recrystallization temperature of doped tungsten, which zs normally very high, but the recrystallization temperature of electron-be am zone-refined tungsten wzre is slightly raised by conlacl with nickel. Recrystallization can be induced at low temperature by the presence of solid nickel on the surface of doped tungsten wire, but apparently not by exposure to nickel vapors alone. Approximately 200 ppm of Ni dijjused into 10-mil wires at 1200 from a deposit of nickel on the surface produced total recrystallization, whereas more than 600 ppm of Ni could be absorbed frotn a vapor source without altering the fibrous structure of cold-worked tungsten. Once initiated, nickel-induced recrystallization required a continued source of' nickel for propagation of the recrystallization front. The solubility of nickel in fibrous 10-mil W wire was approximalely 500 ppm at 1150' C, and the activation energy for penetration of the recrystallization front was 52 kcal per mole. In many applications the usefulness of tungsten depends on critical control of its structure. Cold-worked tungsten with the fibrous structure developed by suitable thermo-mechanical treatment has a low, but technologically significant, ductility. It has long been known1 that traces of nickel, and perhaps other metals, are profoundly deleterious in doped tungsten, because they induce recrystallization at low temperature, which produces a brittle, equiaxed grain structure. This effect appears to be an exception to the general observation that recrystallization is impeded and the recrystallization temperature raised by the presence of impurities.2"9 Previous studies7-'' of the annealing and recrystallization of tungsten wire have divided the phenomenon into prior recovery stages, primary recrystallization and secondary recrystallization. The present investigation is concerned principally with primary recrystallization which is defined here as the replacement of the fibrous structure of deformed tungsten by equiaxed grains. The objective of this study was to explore the nickel-induced recrystallization reaction in tungsten and attempt to elucidate its mechanism. As well, an effort to define which other elements give rise to low-temperature-induced recrystallization was carried out. EXPERIMENTAL PROCEDURE The procedure adopted for these experiments was essentially to bring nickel and other elements into diffusive contact with cold-worked tungsten wires. The process of recrystallization was followed as a function of time and temperature by light and electron microscopic observations. First the influence of nickel on the recrystallization temperature of arc-melted, zone-refined, and variously doped tungsten wire was determined by electroplating a deposit of nickel on the surface of the wire and annealing at a variety of temperatures for 3 hr. The chemical analyses of the tungsten wires used in this investigation are given in Table I. The surface of the tungsten wire was etched with Murakami's slution' and approximately 0.005 in, of Ni was deposited from a Watts-type low pH bath14 for the conditions of these experiments. Variations in plating thickness from about 0.001 to 0.005 in. had no discernible influence on the resulting structures. The wires were then annealed in an atmosphere of dry hydrogen to establish the recrystallization temperature. Concurrently, un-plated specimens were annealed to establish the recrystallization characteristics of nickel-free wire. The criterion of recrystallization was that the fibrous structure be completely replaced by equiaxed grains after a 3-hr treatment of temperature. This provided more reproducible results than use of the first recrystallized grain or a fixed proportion of re-crystallized structure as the critical observation. The structures encountered in longitudinal and transverse sections were examined by both light and electron microscopy at magnifications up to X32,000 using parlo-dion-carbon replicas shadowed with platinum for the latter method. Second, the influence of a variety of metals on the recrystallization temperature of 0.010 in. D alumina-silica doped tungsten wire, AW136-64, was determined. The elements were applied by electroplating whenever possible. Alternatively, they were vapor-plated on the tungsten wire and a greater thickness built up by coating with a dispersion of metal powder in nitrocellulose lacquer. Elements not amenable to either of these procedures were merely slurry coated on the tungsten. The recrystallization temperature was determined as above. Third, the nickel-induced recrystallization process in doped wire was studied more closely by electroplating 8 mils of Ni on 65-mil alumina-silica doped tungsten wire, AW153-NS10, and exposing the wire to temperatures of llOO°, 1200°, or 1300°C for various times in a hydrogen atmosphere. A circular recrystallization front, 'Onsisting of equiaxed grains, developed at the periphery Of the coated tungsten wire, and the advance of this front into the fibrous interior was studied. These experiments employed relatively coarse 0.065 in. D wire because the 0.010 in. D wire recrystallized too quickly to permit observation of the pene-

Jan 1, 1969

THE education of adolescents to perform the duties and assume the responsibilities of maturity has been a characteristic of human society since the dawn of history. In the beginning the members of the immediate family performed this function, and in modern life they still have an important part in it. Possibly religion was the first field in which education began to be functional; young people were sent for instruction to a teacher who had a broader and deeper knowledge of the subject than was possessed by the family. It does not seem necessary for our purpose to attempt to determine how, when, or where instruction in the practical arts first began to become functional, and the brief outline which follows must suffice. The discovery and utilization of mineral substances to improve and maintain the conditions of human living is a practical art, which must have had an almost accidental origin and have been developed by empirical experiments. We do not know, nor would it be useful to try to fancy, how men first learned that they could make use of mineral substances to their benefit, but however that knowledge was initially gained it was certainly trans- mitted through instruction in the family. At fist such activities must have been merely a minor part of the making of a living, bit in time those who excelled found it better to devote them-

Jan 1, 1941

By E. M. Wise

MANY of the platinum metal alloys are hot-forged in the early stages of reduction from ingot and substantial quantities of platinum alloys are commercially employed at very high temperatures in ammonia oxidation units, orifices for forming glass rods and fibers and as cathodes in long-life thermionic amplifiers. They are used also for electrical heating resistors, safety blowout disks, thermocouples and crucibles. The tensile prop-erties at elevated temperatures are important in many of these situations but data on the subject are limited. Creep data also are important, but will not be covered at this time. SCOPE AND CONCLUSIONS Tensile tests were carried out at room temperature and elevated temperatures up to 1100° C. on previously well annealed samples of platinum, palladium and several of their important alloys with composi-tions shown in Table 1. The results are presented graphically in Figs. 1 to 4. The tensile strengths of platinum and the platinum-base alloys (with the exception of the 10 per cent rhodium-platinum alloy) at 1100° C. are from 16.6 to 18.8 per cent of the strengths of the same alloys (well annealed) at room temperature. The strength ratio of the 10 per cent rhodium-platinum alloy is 22.3 per cent, which is appreciably higher than that of the other materials tested.

Jan 1, 1938

By Sidney Cornell

THE technical- advantages of adding oxygen to air and producer gas, or using it as a reactive agent, producing 400 B.t.u. gas instead of. the present 150 B.t.u., with higher flame temperatures and a reducing flame possible, with a smaller volume of gases passing through a furnace, will result in quicker melting, sharp working, and the production of a higher quality steel. Probably electric-furnace quality steel can be produced in an open-hearth furnace using oxygen. A modern, standard, 100-ton open-hearth furnace, with all equipment, costs from $350,000 to $500,000; there are about 1000 open-hearth furnaces in this country. When considering the use of oxygen in the open-hearth furnace, it is necessary to study: (1) The use of oxygen in the present furnaces, such that modification of existing furnaces and equipment cost the minimum, although the full advantages of oxygen are not thus obtainable. (2) The use of oxygen in a furnace designed for its use, producing quality and quantity steel at the lowest possible cost. This entails the junking of approximately one-half the value in existing equipment-writing off $250,000,000. The basis of such an estimate is the present cost of manufacturing open-hearth steel. Objection may be taken to some of the unit prices here given, but while some companies obtain their ores for much less, the prices quoted are -market price. They are used to show the maximum economy obtained by oxygen at that point.

Jan 11, 1924

SLAG composition, slag constitution, reactions in slag, and reactions between slag and metal-in other words, the physical chemistry of slags-are matters of great importance to the open-hearth operator, whether or not he makes use of any detailed knowledge of them. Although this is a relatively young branch of the science of steel- making, much progress has been made; however, much remains to be learned, and many of the statements that can be made at present are probably--or even certainly-subject to future change. Nevertheless, the physical chemistry of slags is sufficiently developed to provide a reasonably secure basis for real understanding of steelmaking reactions. FUNDAMENTALS OF SLAG CONTROL By way of introduction, some time is spent in this chapter on effecting an easy transition from some of the more "practical" manifestations of slag to discussions couched in the more formal language of physical chemistry. This necessitates a certain amount of repetition, but it is felt that the purpose of the chapter is best served in this way. Reactions in the metal phase have products that find their way into the slag and are important components thereof; they are discussed in detail in the preceding chapter. Some substances distribute themselves Between slag and metal in definite fashion, and others are found only in the slag. Their reactions are a large reason for this chapter. Limitations of Slag Control. The open-hearth process is essentially oxidizing and cannot be otherwise operated. (Oxygen gradients in the furnace, the mechanism of oxygen inflow, and similar subjects are discussed in Chapter XIX.) As shown in the calculations of material and heat balances for the charge (see Chapter XV), from 25 to 50 lb. of oxygen will flow from air or combustion gases into the charge or molten bath during the heat for each ton of liquid steel

Jan 1, 1944

The Library of the above-named Societies is open from 9 A.M. to 10 P.M. on all week-days, except holidays, from September 1 to June 30, and from 9 A.M. to 6 P.M. during July and August. The-Library contains about 55,000 volumes, including sets of technical periodicals and the publications of scientific and technical societies. Members of the Institute, with few exceptions, are forced to spend .a portion of their time in localities isolated from sources of information. To these the Library can render valuable service through correspondence; letters requesting information will receive special attention. The Library is prepared to furnish references and copies of articles on mining and metallurgical subjects; to determine the existence of mining maps, and to furnish general information as to the geology and mineral resources of all countries. All communications should be made as definite as possible so that the information received may be what is desired and not include collateral matter which may not be of interest. The time spent in searching for such collateral matter will be saved, and the information will be sent more promptly and in more usable shape. The members of the Institute can be of service to the Library by forwarding copies of mining reports maps privately issued, and similar material, which will he classified, indexed, and made available to other members. Suggestions for additions to the Library, either by purchase or personal solicitation as gifts, will be welcomed. It is hoped that members while in the city will use the Library freely, and. assurance is given that most careful service will be rendered to them.

Jan 6, 1915

The Library of the above-named Societies is open from 9 A.M. to 9 P.M. on all week-days, except holidays, from September 1 to June 30, and from 9 A.M. to 6 P.M. during July and August. The Library contains about 55,000 volumes, including sets of technical periodicals and the publications of scientific and technical societies. Members of the Institute, with few exceptions, are forced to spend a portion of their time in localities isolated from sources of information. To these the Library can render valuable service through correspondence; letters requesting information will receive special attention. The Library is prepared to furnish references and copies of articles on mining and metallurgical subjects; to determine the existence of mining-maps, and to furnish general information as to the geology and mineral resources of all countries. All communications should be made as definite as possible so that the information received may be what is desired and not include collateral matter which may not be of interest. The time spent in searching for such collateral matter will be saved, and the information will be sent more promptly and in more usable-shape. The members of the Institute can be of service to the Library by forwarding copies of mining-reports, maps privately issued, and similar material, which will be classified, indexed, and made available to other members. Suggestions for additions to the Library, either by purchase or personal solicitation as gifts, will be welcomed. It is hoped that members while in the city will use the Library freely, and assurance is given that most careful service will be rendered to them.

Jan 2, 1914

The Library of the above-named Societies is open from 9 A.M. to 9 P.M. on all week-clays, except holidays, from September 1 to June 30, and from 9 A.M. to 6 P.M. during July and August. The Library contains about 55,000 volumes, including sets of technical periodicals and the publications of scientific and technical societies. Members of the Institute, with few exceptions, are forced to spend a portion of their time in localities isolated from sources of information. To these the Library can render valuable service through correspondence; letters requesting information will receive special attention. The Library is prepared to furnish references and copies of articles on mining and metallurgical subjects; to determine the existence of mining-maps, and to furnish general information as to the geology and mineral resources of all countries. All communications should be made as definite as possible so that the information received may be what is desired and not include collateral matter which may not be of interest. The time spent in searching for such collateral matter will be saved, and the information will be sent more promptly and in more usable shape. The members of the Institute can be of service to the Library by forwarding copies of mining-reports, maps privately issued, and similar material, which will be classified, indexed, and made available to other members. Suggestions for additions to the Library, either by purchase or personal solicitation as gifts, will be welcomed. It is hoped that members while in the city will use the Library freely, and assurance is given that most careful service will be rendered to them.

Jan 4, 1913

By P. E. Senseny

INTRODUCTION Massive hydraulic fractures have been used since 1949 in the petroleum industry to enhance production rates and increase recoverable reserves. Currently, a research program, the Multi-Well Experiment, is underway to develop the understanding and technology to a1 low economic production of the large gas reserves of the low permeability, lenticular sandstone formations in the western U.S. (Atkinson, et al, 1981; Northrop and Sattler, 1983). Use of state- of-the-art hydraulic fracturing techniques is a part of this investigation. As a portion of an extensive core program in support of this experiment (Sattler, 1983), fracture toughness has been determined for 56 sandstone, shale, mudstone, or siltstone horizons from three wells in the Piceance Basin. The role of fracture toughness in hydraulic fracturing is not well understood because other factors, such as in situ stress, dominate fracture geometry and containment. Rubin (1983) concluded from analysis of his laboratory hydrofracture experiments that fracture toughness should be included in design and numerical simulation of hydraulic fractures. However, van Eekelen (1982) contends that the stress intensity at the crack front should be so much greater than the fracture toughness of the rock that toughness can have no importance. Generally, fracture toughness and other material properties, such as elastic moduli and permeability, are thought to be of secondary importance in determining fracture geometry and containment. In spite of this, there is a need to acquire a more quantitative understanding of their importance for accurate design and simulation calculations. Analysis of fracture geometry and containment data from hydraulic fracturing experiments carried out in formations where fracture toughness and other rock properties are

Jan 1, 1984

By Will Clark

HE who enters a mining claim within an Indian reservation of the United States of America acquires no rights thereby, because of the fact that the lands within such Indian reservation are not a part of the public domain, and cannot be located or acquired as mineral land. However, where such an entry is authorized as to a particular reservation by an Act of Congress, such claims as may be entered under such authorization are thereby segregated from the reservation, and the Indian title is extinguished. Under the Choctaw Constitution, any citizen of that nation, in other words any Choctaw Indian, who discovered a coal mine, acquired an exclusive right to all coal within a radius of 1 mile. The laws of the Chickasaw nation provided for the formation of corporations to develop coal and other mines, with authority to contract with others to develop and work the mines. Under these laws, leases were made; but Congress subsequently abrogated all existing leases, prohibited all persons from receiving royalties from such mines, and provided that all coal within the nation should remain the common property of the tribes. Such leases are now expressly prohibited by an Act of Congress (32 United States Statutes at Large, 655). All leases of mineral lands upon Indian reservations must now be made under regulations promulgated by the Secretary of the Interior, and the royalties must be paid into the United States Treasury for the benefit of the tribes. In Canada the Indians have no rights to the royal mines and minerals, and the government can make no stipulation with the Indians which would affect the rights of the Province in which the lands are situated. Therefore, while it is true that under our present law no rights can be acquired to a mining claim within an Indian reservation, it seems to be fully within the authority of Congress to make laws, giving such rights to mineral locators as it may deem necessary or expedient.

Jan 6, 1914

By W. R. Hibbard

The increased strength of a polycrystal-line metallic aggregate compared with that of its individual crystals generally has been associated with complex stress distributions at the grain boundaries resulting from atomic irregularity between grains. This disregistry, together with the necessity for adjacent crystals to deform compatibly regardless of the single crystal crystallo-graphic strain mechanism, complicates this mechanism so as to increase the metal's resistance to deformation. Although Taylor1 has shown from purely mechanical considerations the requirement for at least five active slip systems to absorb the complexities during the homogeneous deformation of polycrystalline face-centered cubic metals, experimental studies by Barrett and Levenson2 indicate that this is feasible only in a qualitative sense because of deviations from homogeneous deformation. Seitz and Read in their review3 state: " Unfortunately . . . present knowledge of the grain boundary influence is not sufficient to complement the work in single crystals and provide us with a good foundation for treating polycrystals." The purpose of this investigation was to attempt to clarify the gap between single crystals and crystalline aggregates by an analysis of the effects of dcformational stresses. Some of the results were described by C. H. Mathewson in his 1943 Campbell Memorial Lecture.zl Previous Investigations Since the performance of single crystals deformed under pure stresses has been relatively thoroughly investigated, the most significant researches are concerned primarily with deviations from single crystal behavior of large grained specimens. Qualitative grain boundary effects involving the observed amount of slip werc reported by Carpenter and Elam5 in 1921. Individual crystals in a two or three grained aluminum specimen deformed by tension acted in the normal manner described by Taylor and Elarn4 except for marked modifications at the grain boundaries. There the power to withstand deformation was considerably increased, leaving a ridge on the specimen where decreased slip occurred, often noticeable yi in. from the boundary. Adcock,6 Yamaguchi,' Seumel, Hirstg and others have also reported this phenomenon as a qualitative trend. Yet attempts by O'Neill'o and Ljunggrenll to measure a difference in hardness at grain boundaries in undeformed specimens were unsuccessful. Miller12 measured quantitatively the reduction in slip near the boundary between the single crystal and polycrystalline areas of zinc specimens. These effects consisted of two parts: I. Next to the polycrystalline interface thc distribution of stresses was so altered

Jan 1, 1949

By Robert M. Dreyer

During the past two decades, synthetic abrasives have taken over successively greater percentages of the high-grade abrasive market, so that now, with the exception of natural diamonds (discussed in section 3.15.4C of this chapter), the importance of natural high-grade abrasives is negligible. The predominance of synthetic abrasives is indicated in Table 15.4A.1. This shows that the 1968 value of domestically produced synthetic abrasives (excluding synthetic diamonds) was over $80 million, whereas the value of garnet, the largest domestically produced, natural high-grade abrasive, was less -than $2 million. The major synthetic abrasives (other than synthetic diamonds) are: alumina, silicon carbide, boron carbide, tungsten carbide, and metallic oxides, including various iron oxides. A major advantage of synthetic abrasives is that the size and shape of grain can be closely controlled during manufacture. Although Table 15.4A.1 gives the average price of synthetic abrasives, such averages are of somewhat limited value. This is because the actual price varies within wide limits, depending on composition, hardness, size, and shape of grain. In 1968 the approximate total consumption of abrasives in the United States was valued at about $200 million, of which about two-fifths was in the form of synthetic abrasives (other than diamonds), one-third in synthetic diamonds, and the remainder in natural diamonds. Natural abrasive products, such as silica sand, tripoli, and pumice, are important in the low-cost abrasive field. Of the low-cost abrasives, silica sand continues to be the most important, with domestic production of about 300,000 tons at a value of $1.8 million (see Table 15.4A.1). In general, the lower the sales price of the abrasive product, the more limited is the market which can be served from a given production center. Each abrasive has applications for which it is especially useful, but there is a continual struggle among abrasive suppliers to induce substitution of one product for another. Such substitution can be stimulated by changes in method of preparation affecting hardness, shape, and size of grain.

Jan 1, 1976

By G. H. Gronhovd, W. H. Oppelt

Complete gasification to produce synthesis gas for manufacture of synthetic chemicals and fuels offers possibilities for utilization of the vast lignite fuel deposits in the U.S. The design of a slugging, fixed-bed, pressure gasification pilot Plant is described. Results are presented for initial operation of the plant at moderate pressure and using low-temperature char as fuel. Gasification of solid fuels is becoming increasingly important in the future overall energy picture, both in this country and abroad. Snythesis gas from gasification of coal consists chiefly of carbon monoxide and hydrogen, and after suitable purification and modification this gas can be used in the production of synthetic ammonia, methanol, higher alcohols, and synthetic liquid fuels, or as a reducing gas in the metallurgical field.' Most synthesis gas used in this country is made from natural gas, petroleum oils, and refining tail-gases, but the direct gasification of coal will become more attractive as costs of petroleum oils and natural gas increase.' A gasification process designed for use with brown coal and lignite was developed by the German Lurgi Co. prior to World War 11. In this process a fixed bed of lump-sized fuel is gasified with steam and oxygen at pressures ranging from 370 to 440 psi. Effective heat exchange between the ascending high-temperature gases and the descending solid fuel results in low gas outlet temperatures, high thermal efficiency, and favorable oxygen consumption. Lurgi gasifiers are used commercially for the production of synthesis gas or as a substitute for coal gas in many countries, including Germany, Czechslovakia, Great Britain, South Africa, Australia and Pakistan.3-6 The chief disadvantage of the conventional Lurgi gasifier which operates under nonclinkering conditions is that large quantities of excess steam must be supplied with the oxygen-steam mixture to reduce the temperature in the fuel bed below fusion temperature of the ash. Most of the steam leaves the gasifier undecomposed with the product gas and, after cooling, produces large amounts of dilute liquor. Evaluation of fixed-bed gasification experiments using dry-ash removal indicated that by increasing the oxygen concentration in the oxygen-steam blast the temperature in the combustion zone could be raised high enough to operate under slagging conditions. 7-8 Operation of a fixed-bed pressure gasifier under slagging conditions would reduce the steam requirements and the volume of waste liquor and would increase the steam decomposition, the overall thermal efficiency of the process, and the rate of gas production per unit cross sectional area of the gasifier. Because the Lurgi gasification process, modified for slagging operation, offered possibilities for efficient gasification of American lignite, the Bureau of Mines decided to investigate the process on a pilot-plant scale at the Grand Forks, N. D., Lignite Research Laboratory. DESIGN Description of Pilot Plant: A flowsheet of the Grand Forks slagging gasification pilot plant is presented in Fig. 1. The gasifier unit consits of the coal lock, the gas generator, and the slag lock. The fuel, which is periodically charged to the coal lock, moves by gravity flow into the generator and is continuously gasified by an oxygen-steam mixture introduced at the bottom of the gasifier. Molten slag is formed at the hearth and flows through a central taphole into a water quench bath. The slag-water slurry is periodically discharged from the slag lock. Process steam is generated and superheated in separately-fired, oil-burning units. Oxygen is supplied to the gasifier from a gas storage bank located some distance from the pilot plant. The capacity of the oxygen storage bank is about 130,000 standard cu ft at 2200 psig. Liquid oxygen is delivered by truck and is converted to gas during the filling operation. The superheated steam and oxygen are metered separately, then mixed and fed to the gasifier tuyeres. The gas generator is surrounded by a water jacket. The steam formed is separated in the steam drum and then discharged to the gas offtake, thus equaliz-

Jan 1, 1961

By S. R. Goodman, Hsun Hu

The rolling texture transition in copper as a function of deformation temperature is found to be quite similar to that in high-purity silver. The ordinary copper type texture changes gradually to the brass type, accompanied by an increase in the stacking fault frequency, as the temperature of deformation decreases. The rolling textures obtained at low temperatures and the corresponding annealing textures compare remarkably well with the ordinary rolling and annealing textures of low-zinc brasses. Furthermore, it is also found that the observed stacking fault energies of copper specimens deformed at low temperatures correspond closely with those of low-zinc brasses, as deduced from measurements of the dislocation nodes. These results are consistent with the idea that texture transition may be significantly dependent on the stacking fault energy. It was shown in a series of previous publications1"3 that the rolling texture of high-purity silver changes gradually from the common silver type (or the brass type) to the copper type* with increasing temperature *The silver or brass type rolling textures are commonly described as (110)[112],4,5 whereas the copper type rolling textures are mainly (123) [a121 and (146)[211].5 Other ideal orientations have been used by various investigators for the copper type rolling textures, but the actual difference among these ideal orientations is rather small. of deformation, and that such texture transition can be correlated with the change in stacking fault frequency as a function of rolling temperature. Furthermore, it was shown that the formation of annealing textures in high-purity silver from the various rolling textures obtained during the course of texture transition depends entirely upon the deformation texture. From a common silver type or brass type rolling texture (such as produced by rolling at 0" or at 50° C) the recrystallization texture is mainly (120)[211], which is quite different from the recrystallization texture of brass.* However, for both ma- terials the orientation relationship between the rolling texture and the recrystallization texture can be expressed in terms of similar rotations around [Ill.] axes of approximately 30 or 35 deg. They differ in that the [Ill] rotational axes are different. In the case of high-purity silver, the axes of rotation are the two (111) poles near the plane normal of the deformed specimen with a (11l)[112] type rolling texture, whereas in brass, they are the (111) poles near the direction of rolling. For high-purity silver with a predominantly copper type rolling texture (such as produced by rolling at 150° or 200°C) the recrystallization texture is mainly (100)[001], or the cube texture, plus its twin orientations. It was shown previously6 that such reorientation observed in copper or aluminum can be described as [Ill] rotations of 30 to 40 deg. For intermediate cases, i.e., when the rolling textures are composed of a

Jan 1, 1963

By M. R. Geer

THE increase in the number of coal-cleaning plants employing dense-medium processes occurring since 1946 is especially interesting when viewed historically. Both sand and magnetite were introduced as material for heavy mediums at about the same time, sand in the Chance process in 1921 and magnetite in the Conklin process in 1922, but from that point on their records diverge. The Chance process enjoyed a steady growth from its inception, whereas no additional magnetite plants were built in the United States for over 20 years. Then, following the close of the World War 11, magnetite was again introduced, this time with marked success. During the following years some 47 plants employing magnetite medium were built.

Jan 7, 1953

By C. M. Schwartz, A. E. Austin, W. B. Wilson

High-temperature X-ray diffraction studies were conducted with Th-U alloys with up to 10 wt pet U. The solid solubility of uranium in thorium as a function of temperature was determined by the method of lattice parameters. Thorium will dissolve up to 2.5 wt pet U at 950°, 4.5 wt pet U at 1150°, and 7.5 wt pet U at 1250°C. Determinations were made of the temperature of the transition of thorium and of the effect of uranium upon the transition. The a to ß transition for thorium was observed to occur at 1330' ±20°C. Mean coefficients of expansion were calculated for thorium and two alloys, and for ThO2 in contact with the thorium, using X-ray lattice-parameter data. Values obtained at 950° C for thorium and Tho2 were 12.1 and 9.40 X 10-6 per OC, respectively. Impurities obtained during the X-ray exposure were identified by diffraction and were essentially Tho2 and ThC, with two additional unknown phases being detected. The effect of the impurities upon the results is discussed. DIRECT investigation (i.e., high-temperature X-ray diffraction studies) of the phase diagram of thorium-rich uranium alloys has been shown to be necessary since recent work1 - has disclosed the presence of an allotropic transformation near 1400°C in pure thorium with the room temperature face-centered-cubic phase transforming to a body-cen-tered-cubic structure at the elevated temperature. The effect upon the transition of the addition of uranium to thorium and of the solubility of uranium in thorium at high temperatures remained unknown, yet was of interest in understanding fabrication procedures and elevated temperature use. The present work was undertaken to provide information in this area by determining the transition temperature, the effect of uranium on the transition temperature, and the solubility of uranium in thorium as a function of temperature. Experimental Work The high-temperature diffraction data were obtained using a camera especially designed for the purpose3 and capable of reaching temperatures in excess of 2000°C at pressures as low as 1 x 10." mm Hg. Temperature regulation was provided by regulating the power input to ±0.1 pet variation, and by regulating the water flow through the camera jacket to provide a constant thermal load. The X-ray sample was a rod nominally 80 mil diam, which was further turned down to 20 mil and then etched to 18 mil over 1/2 in. of one end. This was placed in the sample holder and mounted on the camera so that the smaller part was surrounded by a cylindrical tantalum-sheet radiation-type heating element. Diffraction from the sample was recorded on film after passing through a slot in the heating element and radiation-baffle shield and through beryllium vacuum windows. The X-ray film mounting was of the Straumanis type4 with a camera diameter of 114.59 mm. Since previous work of Chiotti' indicated that impurities considerably alter the transition temperature, chemical analysis of the arc melted iodide crystal-bar thorium samples was obtained prior to testing. The analysis disclosed the material to contain as low as 0.001 ±0,0002 wt pet H and 0.007 ±0.001 wt pet 0. Carbon was 0.003 wt pet and nitrogen less than 0.002 wt pet. This material was sealed in mild steel in an inert atmosphere and subsequently hot rolled to 3/8-in. diam rods at a temperature of 732°C. Following removal of the jacket, the material was pickled and cold swaged to 1/8-in. rods, from which the diffraction samples were prepared. The alloys were similarly prepared, with the uranium being added during arc melting. The uranium analyses of the alloys prepared appear in Table I. The experimental procedure for diffraction examination of the three samples of high-purity thorium differed from those of the Th-U alloys. The original practice, later modified, consisted of pumping down the camera with the diffusion pump on and then admitting liquid nitrogen to the cold trap of the system. This was modified for the Th-U alloys by maintaining liquid nitrogen in the cold trap at all times before and while the diffusion pump was heated. This minor change produced a reduction in the amount of carbon pickup by the sample during exposure to the diffusion-pump vapors. The sample was brought to the desired test temperature and exposed for 21/2 hr at pressures which were usually 2 x 10-6 mm Hg, or lower. Exposures were made at

Jan 1, 1959

By R. H. Hopkins, R. W. Kraft

X-ray and metallographic analysis reveal that the preferred cryslallograPhic relationships in direc-tionally solid~fied Pb-Sn eutectic specimens can be stated: interface growth direction, Experiments in which tin single-crystal seeds were used to nucleate the eutectic demonstrate that the normal lamellar structure observed at steady state can be forced to break down initially to a semide-generate structure when the crystallograPhic direction of the tin seed does not lie within the preferred eutectic interface plane. A normal structure eventually develops by preferred grain growth. X-ray topo-graphs and rocking curves substantiate that the perfection of eutectic samples increases as growth proceeds until steady-state conditions prevail. RECENT years have seen substantial progress made in the understanding of eutectic solidification through both intensive theoretical1'' and experimental investigations (see Ref. 7 for a review and extensive bibliography of both aspects). Several important observations concerning the nucleation and growth aspects of binary eutectic solidification have been brought to light. Briefly some of these include the nonrecipro-cal nucleation of one phase upon another,'j9 the tendency for a specific low-index direction of one or both phases of the eutectic to be aligned in the growth direction during unidirectional solidification,'0711 and the production of lamellar microstructures having a preferred interface plane between "11-13 phases. Questions quite naturally arise as to the mechanism by which preferred grain growth evolves during eutectic solidification and what relationships (if any) connect the initial nucleation of one phase upon another with the preferred growth directions and interface planes observed after a few centimeters of growth in many systems. This study was initiated in an attempt to answer these questions. An experiment was devised in which both the nucleation and growth steps in the crystallization of a binary eutectic, Pb-Sn, could be correlated with subsequently developed eutectic morphology and crystallography. This was accomplished by nucleating the eutectic upon a tin single crystal seed and then causing the eutectic to grow from the seed by directional freezing. The morphology of the structures produced in this manner was then monitored metallographically and the orientation relationships and substructural perfection determined by X-ray analysis. The information thus ob- tained was correlated to the growth history of the samples. EXPERIMENTAL DETAILS The eutectic of composition 38.1 wt pct Pb and 61.9 wt pct sn14 was prepared by accurately weighing lead and tin of 99.999+ (from ASARCO and Lytess Metals and Chemicals, respectively), melting in a clean Pyrex beaker under an argon blanket, and casting into the proper crucible for resolidification as described below. Tin seeds were grown by the method of ~halmers," saw-cut, oriented by the Laue method, and soldered to the pull rod of the Czochralski puller. All seeds were given a final electropolishing (to assure the removal of any deformed material from the cutting operation) and acetone degreasing immediately prior to the nucleation experiment in which they were to be used. Eutectic samples were unidirectionally solidified in a horizontal graphite boat1' or by pulling from the melt16 with tin (or graphite) seeds. A flowing argon atmosphere was employed in all experiments and growth rates and temperature gradients, constant for a given run, varied from 2 to 4 cm per hr and 8" to 15°C per cm over the course of all the experi-

Jan 1, 1969

By T. Gleason

Problems involved in applying wet scrubbers to gas cleaning coal dust from thermal dryers are reviewed. Careful consideration of all the elements going into a modem coal preparation plant is required in view of the increasing difficulty of applying suitable gas cleaning equipment. This problem arises not only from the presence of finer coals to be handled, but also from the pressures applied by both the general population and the plant operators to improve the standard of gas cleaning performance. The Peabody scrubber is presented by the author as a machine designed to help improve this cleaning operation. Wet scrubbing of fine coal from thermal dryers poses a number of problems in adapting the gas cleaning equipment to the fine particulate matter. Among them are: 1) Dust in gases leaving the thermal dryer cyclones is often extremely fine with high percentages of total dust loading less than 1p in size. 2) Flue gas entering the scrubber is corrosive since the coal fired in the thermal dryer furnace is in the range of 0.7% by weight sulfur or higher. Therefore, comparatively high cost stainless steel alloys or corrosion resistant linings are required for a satisfactory service life. 3) Requirements for residual coal loadings leaving the gas scrubber are continually being lowered, while modern coal preparation operation is imposing heavier burdens on the collection system through introduction into the thermal dryer system of very fine coal previously not recovered. The advent of flotation systems in increasing numbers is typical of this trend. 4) Installation of a scrubbing system on thermal dryers is made primarily to reduce air pollution and product recovery value is of little or no value. Therefore, the operating costs of gas pressure drop and water requirements must be held to a minimum. We have, then, the basic situation which calls for comparatively high cost stainless steel alloy wet scrubbers, which must be highly effective in removing coal fines particularly in the 0 to 5-p size range. Further, the standards of scrubber performance are continually being raised towards the level where gas discharged from the scrubbers must be essentially free of any coloration due to residual dust. In view of the highly refractive nature of fine coal dust, residual loadings of 0.01 grains per cu ft or less are required to provide a color free discharge gas. In the present specifications under consideration a residual coal loading of 0.05 grains per cu ft would be considered color free, since the discharge gases are saturated in the range of 150°F. The steam plume acts as a masking agent at the point of discharge, and upon dissipation of the 150° saturated vapor stream, the effluent gas stream could be essentially color free. The specification under consideration calls for residual solids loading of 0.05 or less grains per cu ft, given a coal size distribution shown in the basic data in Table I. It is noted that the dust laden coal stream has a size distribution by weight of 33% in the 2 to 5-p size range and 55% in the 0 to 2-p size range. The particle size distribution given in the specifications does not detail the percent by weight less than 1-p in size, and more important, the size distri-

Jan 1, 1963

By Donald H. McLaughlin

THE primary function of the mining engineer is to find mineral deposits and fuels in the accessible rocks of the earth and to recover them for the vast needs of our complicated civilization. On him has been placed the responsibility for the exploitation of the nation's and world's mineral resources. The degree to which the minerals of the earth have been utilized serves to an extent as a measure of man's material advancement, as well as an index of the relative strength of nations. The natural endowment of lands, varies greatly, but the intellectual energy of a people is revealed by the way in which they take advantage of their heritage of minerals or reach out to less developed regions by exporting their engineering skill as well as capital to secure the raw materials they need.

Jan 2, 1953