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By J. Grosso, D. J. Nagel

In many metallurgical studies, it is necessary to reveal the composition and structural properties of materials. Usually this is done by etching, but some substances do not etch well or easily. Anodizing is known to provide an alternate treatment in many cases. In general, this technique is simple, often more sensitive to composition differences than etching, has excellent resolution, and provides variable contrast in those elements and alloys which anodize. Here we report the use of anodizing in diffusion studies in the TiCb system. Fig. 1 shows a cross section of the diffusion zone in a TiCb couple. The anodizing has clearly revealed both composition and crystallographic features. The maximum bulk penetration of the titanium into the columbium is marked by a sharp line because of the steep concentration gradient. The titanium grain size and orientation differences are also evident. Variation in the grain size reflects the gradually decreasing columbium concentration.

Jan 1, 1967

By Rudolph G. Wuerker

MUCH descriptive matter[ ] has appeared on the subject of suspension roof supports, or roof bolting, as it is more commonly called. The wide- spread introduction of roof bolting into coal mines and metal mines is truly phenomenal. Mine operators were quick to recognize the advantages of supporting wide openings without hindrance to machine maneuverability and ventilation.

Jan 6, 1953

By M. C. Udy, C. H. Lorig

THROUGH the years much interest has been centered in attempting to develop a direct method of iron-ore reduction, to replace or supplement the present indirect blast-furnace process. It would not be difficult to produce a list of more than 500 patents dealing with the direct production of iron and steel, but the few of this type of process that have proved successful do not produce in competition with the blast furnace; they produce special products. A survey of the literature reveals that the equilibrium conditions for the reduction reactions (iron oxides with carbon monoxide and with hydrogen) have been fairly well established but that data on the rate of reaction are discordant, although the general effects of the variables are known. This dissertation deals with the rate of reduction of a magnetite concentrate with hydrogen. The following variables have been studied: bed depth, gas velocity, particle size and temperature. The behavior of a single particle was also studied. LITERATURE Two general factors should be considered in a study of reduction of iron oxide: (I) equilibrium relations, and (2) rate of reaction. The first factor, equilibrium, has received the attention of many investigators and the equilibria Fe304-FeO-H2-H20, Fe3O4-FeO-CO-CO2, FeO-Fe-H2-H20, FeO¬Fe-CO-C02 are fairly well established. Of the second factor, the rate of reaction, much less is known. Data are comparatively scarce and there is very little concordance. The discordance probably results from the large number of variables influencing the reactions. However, the general effect of the variables is known. Among these variables are temperature, gas velocity, particle size, porosity, gas composition (distance from equilibrium), presence of impurities, greater or less prevalence of side reactions, and even design of the apparatus itself. Wetherill and Furnas1 published an excellent paper in 1934. They point out that any one or more of five processes (the chemical reaction, diffusion of the reactant through the gas film, diffusion of the reactant through the solid phase, diffusion of the reaction product through the solid phase, or diffusion of the reaction product through the gas film) may be the slow process, and thus the rate-controlling process. It is regretted that the work of these authors was limited to experiments at one temperature, and that the range of gas compositions was limited. Langmuir2 has shown that heterogeneous reactions take place at phase boundaries.

Jan 1, 1942

By E. A. Gulbransen, J. W. Hickman

ONE of the important factors that determine the resistance of a metal or alloy to further chemical reaction is the structure of the superficial oxide film A thorough understanding of the physical and chemical structure as well as the stability of the oxide film formed on the surface as a function of time and temperature of the chemical reaction might furnish clues as to the nature of the reaction process and the protective nature of the film A comprehensive program has been undertaken to study these phenomena This paper summarizes the structure of the oxide films formed on the metals iron, cobalt, nickel, chromium and copper at temperatures up to 700°C Before the introduction of the electron diffraction technique, it «as necessary to use either direct chemical analyses or X-ray diffraction analyses to determine the nature of the oxide film formed on the metal or alloy Chemical analyses yields information on the percentages of the several atomic species present in the film while X-ray diffraction analyses yield information on the atomic geometry In special cases the information obtained may be identical, but in general both view-points are necessary Much of, the early work was carried out on the oxidation of bulk samples where thick films were obtained The products were identified after cooling to room temperature by X-ray diffraction and chemical analyses Although much useful information has been obtained in this manner, little could be learned about the character of the protective oxides during the period when the films were actually protective Evidence concerning the chemical structure of thin oxide films has been made possible by the development of the electron diffraction reflection technique In this method the most fruitful investigations have been made by carrying out the reaction in situ at the temperature at which the film is actually protective LITERATURE The oxidation of iron has been extensively investigated by X-ray and electron diffraction Jackson and Quarrell1 found that oxide films formed and examined at the same temperature differed considerably from those allowed to cool to room temperature The results showed that below 400°C the oxide that was stable in intimate contact with iron was Fe304, between 515° and 900°C the stable film was FeO Above the upper change point of iron the oxide was found to be Fe304 prom 400° to 515°C , FeO, Fe304 or a mixture of the two oxides was found Recrystallization of the air-formed film below 400° and above 900°C led to the formation of Fe304 In the range where thicker films consisted of FeO, the air-formed film was converted to a new hexagonal oxide not previously described

Jan 1, 1946

By Craig S. Hartley

Expressions are obtained for the energy changes associated with the reaction of (a& (111) slip dislocations on intersecting (110)planes in anisotropic bcc metals. An energy criterion for assessing the likelihood of dissociation of the products of such reactions is also presented. It is found that the "burrier reactions" which form a(100) dislocations at the intersection of two active {110) slip planes are more energetically favorable in metals which exhibit a high value of Zener's anisotropy factor, A, than those which have a low value. The results are presented in a form which permits the stacking fault energy to be obtained from a measurement of the separation between par-tials in a dissociated configuration. However, until accurate calculations or measurements of the stacking fault energies involved are available, it is not possible to assess the physical importance of dissociated dislocations. In a recent paper,' the energy changes associated with several types of reactions between two slip dislocations, (a/2)(111){110), in bcc structures were calculated.* Isotropic elasticity and the approxima- tion v = -3- were employed. The purpose of this work is to present calculations of the energy changes for many of the same reactions using anisotropic elasticity. The problem of dissociation of a(100) and a(110) dislocations is also considered, and maximum fault energies for which dissociation will be energetically favorable are calculated for several bcc metals. Two general types of reactions are considered; those for which the reactant (a/2)(111) dislocations have long-range attractive forces and those for which the reverse is true. An example of the former is: (a/2)[lll] + (a/2)[lll]-a[l00] while the latter are typified by: (a/2)[lll] + (a/2)[111] -a[011] Only reactants lying in different slip planes are considered; therefore, the products must lie along (111) or (100) directions, which are the intersection of two {llO} planes. It will be assumed that the reactants and products are infinitely long parallel dislocations, since in this case the energy change associated with the reactions is a maximum.' THEORY The self-energy per unit length of a straight mixed dislocation in an anisotropic medium can be written? where b is the Burgers vector, K is an appropriate combination of the single-crystal elastic constants, and R and ro are, respectively, outer and inner cut-off radii of the elastic solution. The energy given by Eq. [I] does not account for any variation of the core energy with orientation. This could be manifested by an orientation dependence of the core radius or, equivalently, the Peierls width, of the dislocation. However, the energy contribution due to this source is expected to be small, and current models of the dislocation core are not sufficiently accurate to justify such a refinement. It has already been shown that for the isotropic case the energy contributions due to nonzero tractions across the cores of the reactants and products exactly cancel one another in the reaction.' Accordingly, it will be assumed that this contribution to the total energy change in the anisotropic case is small. In the subsequent discussion it is also assumed that the core radii of the reactant and product dislocation are the same and that, where stacking faults are formed, the faulted region is bounded by the centers of the partials. Consequently only changes in elastic energy due to the reactions will be considered. When the dislocation is parallel to either the (111) or the (100) directions, K may be written:375 K = (Ke sin2 a + Ks cos2 a) [2] where K, and Ks are the combination of elastic constants corresponding to an edge and screw dislocation lying along the same direction as the mixed dislocation, and a is the angle between the direction tangent to the dislocation line and the Burgers vector. Eq. [2] should not be confused with the isotropic approximation to the variation in energy with line Orientation.6 It should be noted that the essentially isotropic expression for K is a result of the characteristic symmetry of the (111) and (100) directions and is not, in general, valid for other dislocation directions in anisotropic cubic metals. The energy* change for a reaction in which the re- actant and product dislocations are parallel perfect dislocations can be written: where Ep and E, refer to the self-energies of the products and reactants, respectively. For dislocations parallel to (100) and (111) directions, Eq. [3] becomes:

Jan 1, 1969

By J. L. Lamont, W. Crafts

Studies of the effect of composition of steel on hardenability by Grossmann,' and as-quenched hardness by Field2 and by the authors, have made it possible to predict the results of quenching when the composition and cooling rate are known In order to extend the application of the hardenability calculation to the quenched and tempered condition in which steel is finally used, a survey has been made of the hardness changes caused by tempering. From this study a method has been developed for the prediction of hardness and tensile strength of steel in the tempered condition. The method of calculation was developed from Rockwell C hardness tests on quenched and tempered Jominy specimens and is expressed in Rockwell C hardness units. It is of an additive type in which the degree of softening from as-quenched hardness is estimated. Tem-pred properties may be calculated within about plus or minus 5 Rockwell C hardness or plus or minus 15,000 lb. per sq, in. tensile strength. This degree of accuracy is less than that necessary for the control of heat-treatment, but is adequate for the comparative evaluation and selection of alloy steels. The formula indicates that tempered hardness is primarily dependent on as-quenched hardness and, as in the hardening reaction, the progress of tempering is controlled mainly by the carbon content. Alloys tend to retard softening by a secondary hardening mechanism in which the alloy appears to migrate from ferrite to the carbide phase. The factors for the effects of alloys in tempering vary so much from the effects of alloys in hardening that different steels of equivalent hardenability may, after like heat-treatment, differ considerably in tensile strength. Procedure In developing the method for calculating tempered Rockwell C hardness, simple and complex steels were tested over a range from 0.08 to 0'65 per cent carbon and up to 2.68 per cent manganese, 2.18 silicon, 3.50 chromium, 4.94 nickel, and 1.06 molybdenum. The steels were made as small induction-furnace heats at the Union Carbide and Carbon Research Laboratories, Inc' The accuracy of the method was finally checked on a variety of carbon, low-alloy and high-alloy types of heat-treating steels produced under commercial conditions. The method was based on a study of tempered Jominy bars, and its validity was tested by correlation with the center hardness and tensile strength of oil-quenched and tempered bars from 1/2 to 4 in. in diameter. The method of calculation was derived from the differences in Rockwell C hardness between as-quenched and quenched and tempered Jominy specimens. Prenormalized Jominy hardenability speci-menS quenched from a normal temperature for austenitizatios were used to obtain a range of as-quenched Rockwell C

Jan 1, 1948

By W. Crafts, J. L. Lamont

Studies of the effect of composition of steel on hardenability by Grossmann,' and as-quenched hardness by Field2 and by the authors, have made it possible to predict the results of quenching when the composition and cooling rate are known In order to extend the application of the hardenability calculation to the quenched and tempered condition in which steel is finally used, a survey has been made of the hardness changes caused by tempering. From this study a method has been developed for the prediction of hardness and tensile strength of steel in the tempered condition. The method of calculation was developed from Rockwell C hardness tests on quenched and tempered Jominy specimens and is expressed in Rockwell C hardness units. It is of an additive type in which the degree of softening from as-quenched hardness is estimated. Tem-pred properties may be calculated within about plus or minus 5 Rockwell C hardness or plus or minus 15,000 lb. per sq, in. tensile strength. This degree of accuracy is less than that necessary for the control of heat-treatment, but is adequate for the comparative evaluation and selection of alloy steels. The formula indicates that tempered hardness is primarily dependent on as-quenched hardness and, as in the hardening reaction, the progress of tempering is controlled mainly by the carbon content. Alloys tend to retard softening by a secondary hardening mechanism in which the alloy appears to migrate from ferrite to the carbide phase. The factors for the effects of alloys in tempering vary so much from the effects of alloys in hardening that different steels of equivalent hardenability may, after like heat-treatment, differ considerably in tensile strength. Procedure In developing the method for calculating tempered Rockwell C hardness, simple and complex steels were tested over a range from 0.08 to 0'65 per cent carbon and up to 2.68 per cent manganese, 2.18 silicon, 3.50 chromium, 4.94 nickel, and 1.06 molybdenum. The steels were made as small induction-furnace heats at the Union Carbide and Carbon Research Laboratories, Inc' The accuracy of the method was finally checked on a variety of carbon, low-alloy and high-alloy types of heat-treating steels produced under commercial conditions. The method was based on a study of tempered Jominy bars, and its validity was tested by correlation with the center hardness and tensile strength of oil-quenched and tempered bars from 1/2 to 4 in. in diameter. The method of calculation was derived from the differences in Rockwell C hardness between as-quenched and quenched and tempered Jominy specimens. Prenormalized Jominy hardenability speci-menS quenched from a normal temperature for austenitizatios were used to obtain a range of as-quenched Rockwell C

Jan 1, 1948

By John Chipman

IN the manufacture of rimming steel-which constitutes the bulk of the world's production of mild steel-the factors that determine the quality of the product are very closely associated with the pouring and solidification of the steel in the ingot mold. The behavior of the metal in the mold is, on the one hand, the resultant of the complex processes through which the liquid metal has passed, and, on the other, it is an indication of the probable behavior of the ingot during subsequent rolling and finishing operations. A detailed study of the mechanism of solidifica-tion of rimming ingots ought to yield information that will be useful iii controlling the structure of the ingot and the quality of the ultimate product. The first step in such a study is to determine the rate at which the solid shell of the ingot forms from the liquid metal in the mold. A knowledge of the rate of solidification will make it possible to correlate observations of rimming action and gas evolution with studies of the structure, porosity, and segregation within the ingot. Thus, if the metal in the mold is observed to fall, let us say one minute after pouring, the portion of the structure associated with this fall will lie located in the part of the ingot that is solidifying at that particular moment. The knowledge that the ingot solidifies to a depth of ¾ in. in the first minute enables us to locate in the ingot the structural features corresponding to the observed fall. Conversely, the blowhole condition associated with a rising or growing ingot will be found in the part of the ingot that is solidifying at the time the phenomenon occurs. The time required for the complete solidification of an ingot has long been a matter of speculation. It is of considerable practical importance in connection with charging and heating in the soaking pits. Too rapid handling of the ingot through heating and rolling processes has been thought to be associated-with excessive pipe and other internal defects, so that a further object of this investigation was to attempt to estimate the time required for complete solidification, or the minimum practical time within which the subsequent operations can be performed with the minimum hazard.

Jan 1, 1937

By J. A. Herbst

During the last decade it has been established that conventional mineral-processing control strategies based on classical control theory result in significant increases in plant throughput and operating-cost savings. It has, however, also been recognized that conventional strategies have important limitations for complex multivariable mineral-processing systems. These limitations center around the fact that single-input/single- output control linkings often result in highly undesirable interactions between controllers. During the last few years new and promising approaches to solving this problem have emerged. These approaches are based on the use of on-line dynamic models to make predictions which are useful for control decision-making. This paper presents a brief summary of the state-of-the-art for mineral-processing control in 1984. This summary is followed by a review of recent developments in model-based control strategies including those in optimal control, self- tuning regulators and decoupling control. Expected trends for the future in the control of mineral-processing operations are discussed.

Jan 1, 1984

By Gilbert Santoro

In this study tantalum carbide filaments of various compositions in the fcc region were prepared by heating a tantalum wire in a measured amount of hydrocarbon vapor. Such properties as tensile strength, transverse-rupture strength, microhard-ness, lattice parameter, electrical resistivity, and magnetic susceptibility were measured as a function of carbon content. Some of these properties showed a maximum or a minimum between a carbon-to-tantalum molar ratio of 0.80 and 0.85, the composition range at which the color changes from metallic gray to gold. The recent literature has shown that in the large homogeneity range for the fcc phase of the Ta-C system there is a marked variation for such properties as microhardness,' electrical resistivity, ' thermodynamic properties,z'3 lattice parameter and superconductivity. In addition to the technological interest of these variations within a single phase, important theoretical benefits may ensue from a continuous investigation of properties vs stoichiometry in tantalum carbide and other refractory defect compounds, for example the effect of the metal-metal distance and crystal structure upon bond formation and electronic structure. Whether there is a similar variation of the tensile strength is of practical importance. Of theoretical interest would be the knowledge of how the magnetic susceptibility varies with carbon composition. Both of these properties, as well as the transverse-rupture strength, were determined for tantalum carbide filaments in the fcc phase region. The lattice parameter, the electrical resistivity, and the microhardness were also investigated and compared with values appearing in the literature. EXPERIMENTAL PROCEDURE Material Preparation. Tantalum carbide specimens of various carbon content were prepared by statically carburizing high-purity tantalum filaments in measured quantities of pure hydrocarbon gas. The filaments, which were 10 mil in diameter and 20 or 40 cm long, were heated by their own resistance at temperatures from 1800" to 2200°C using alternating current in some cases and direct current in others. Tantalum wire from two sources was used. One had a reported purity of 99.96 wt pct Ta. The ingot from which this wire was drawn had been electron beam-melted as the final step in its purification. The reported purity of the other wire, which was prepared by a powder metallurgical process, was 99.88 wt pct Ta. The impurities of both tantalum sources are listed in Table I. Spec-trographic-grade toluene or research-grade propane was used as the source of carbon. The apparatus for the carburization of the filaments is shown schematically in Fig. 1. The system was evacuated to 1 x l0-' mm of Hg when using the electron beam-melted tantalum and to less than 1 p when using the less-pure tantalum. Neither the difference in the base vacuum, nor in the hydrocarbon gas, nor in the tantalum filaments resulted in any detectable difference in the properties studied in this work. However, only the carbides prepared from the higher-purity tantalum were used in the magnetic-susceptibility determinations. Once the base vacuum had been reached, the system was flushed with the hydrocarbon and re-evacuated. For any desired composition of the carbide, hydrocarbon gas was allowed to leak into a constant-volume flask to a predetermined pressure. These pressures were measured by a Cartesian diver-type mercury gage with a range from 0 to 20 mm and with a scale expanded to nine times. The hydrocarbon gas was allowed into the reaction tube and the filament was quickly raised to the reaction temperature. The slack in the filament due to thermal expansion was taken up by drawing out the movable electrode with a screw mechanism. The filaments were kept at temperature from a few minutes to 200 hr. In the majority of cases the heating time was 6 hr. The reaction tube was cooled by cascading water on its outer surface. By means of an ammeter and a voltmeter the electrical resistance at the reaction

Jan 1, 1963

By Ernst F. Eurich

(Cleveland Meeting, October, 1912.) ALEXANDER PARKES patented in England in 1851-52-53 a process for desilvering lead by means of zinc, making use of the greater affinity of silver for zinc than for lead, discovered by Karsten in 1842. The efforts in England to develop it commercially were not particularly successful, nor was the attempted introduction into the United States. This last was not surprising, as it was about the beginning of our Civil War, and at that period there was very little lead-bullion produced in the united States and there was no field for the process here. There was at that time on Staten Island an establishment that pattisonized lead, probably from Rossie, N. Y., and Chester, Pa., and possibly some Spanish lead, but the production of lead-bullion in the Far West had not yet begun. In 1864, Edward Balbach, of Newark, N. J., patented in this country a process for desilvering lead by means of zinc, and in 1867 Edward Balbach, Jr., patented a " movable black-lead retort with a neck, placed in a furnace," for the purpose of distilling the alloy of zinc, lead, and the precious metals. A brief comparison of the Parkes and the Balbach processes is interesting. The Parkes process as practiced in England consisted in stirring into silver-bearing lead, melted in a kettle, from 1 to 2 per cent. of zinc, cooling, skimming the alloy of lead, zinc, and silver that rose to the surface, liquating it in an iron retort, distilling the residual rich alloy in fire-clay retorts, thus regaining the zinc, and refining the desilvered lead at a low heat in a shallow cast-iron pan that formed the hearth of a reverberatory furnace. If the lead was too impure, it was first softened * Presented also at the Joint Meeting of the Institute and Section IIIa, Metal¬lurgy and Mining, of the Eighth International Congress of Applied Chemistry, New York, September, 1919, and here published by mutual agreement.

Dec 1, 1912

By Nicholas J. Grant, Oliver Preston

PUBLICATION of data by Irmann' indicating outstanding thermal stability and elevated-temperature strength properties in a sintered aluminum powder product (SAP) stimulated interest in the strengthening of metals by means of a highly dispersed oxide phase. This material was produced by compacting, sintering and extruding a fine flake aluminum powder, resulting in a dense product containing 10 to 16 volume pct alumina, which arises from the thin oxide film on the starting powder, highly dispersed in a matrix of pure aluminum. The method of producing SAP, and the stable high-temperature properties obtained from it, introduced the possibility of developing superior materials for high-temperature service by powder metallurgy methods. The composition of the materials of this type which are presently under consideration is predominantly metallic, containing from less than 1 pct up to about 20 volume pct of the oxide. As a result, other properties of these materials, such as electrical and thermal conductivity, thermal shock resistance, and to a certain extent ductility, notch sensitivity, machinability and hot working properties, are also predominantly metallic. These alloys do not constitute, therefore, a completely new class of materials as do the cermets, but rather present a new means of modifying the properties of a metallic matrix. In this sense, SAP type alloys are more closely analogous to the alloy aging systems. While the strength properties realized in the oxide-pure metal systems at the lower temperatures are substantially less than the best attainable in the aging systems, the thermal instabilities in the latter make them of less value for use at temperature much above their optimum aging temperatures, as indicated in Fig. 1. While the means of obtaining an oxide dispersion are more difficult and costly than conventional aging processes, in the light of the as yet limited understanding of such systems there is considerable promise of improved high temperature properties arising from the thermal stability of these structures. Since the development of SAP in 1946, its properties and the properties of a series of similarAl,O,-A1 products containing from about 1 to 20 pct aluminum oxide have been fairly extensively studied and reported.'- "articular attention has been given to

Jan 1, 1958

By C. L. Kinney

The rapid increase in the amount of steel produced by the basic open-hearth process is an index of its ability to produce high-grade steel from raw materials of the most, varied physical character and chemical analysis. This inherent adaptability of the process has resulted in a lack of care in the selection of raw materials, so that in far too many cases charges are used of a chemical and physical character not justified by local economic conditions. A practice, or series of practices, should be used that will result in the greatest economy for the plant as a whole; therefore, the operations of blast furnace and open hearth must be considered together. In this paper, an effort has been made to show those variations in both open-hearth practice and cost that follow changes in the analysis of the pig iron arid it may be said that the theoretical costs shown are worthy of careful study and consideration. Carbon, manganese, silicon, phosphorus, and sulfur constitute the principal metalloids in basic pig iron and play the leading role in the production of steel by the basic open-hearth process. The percentages of each of these metalloids, with the exception of carbon, is a variable that has its genesis in the economic relation of the blast-furnace plant to its ore and fuel supplies. As the amount of carbon in the iron is a saturation function of the temperature at which it is produced, the variation in the amount carried is, for any given locality and grade of iron, practically negligible and is so considered in the eight heats discussed in this paper. The melting and refining reactions in an open-hearth furnace, either acid or basic, are essentially oxidizing and vary greatly with the type and age of the furnace, as well as the character of the fuel employed. The outstanding characteristic of the basic process, and the one that explains its predominance over the acid, is its ability to form out of the lime charged and the phosphorus oxidized from the charge a stable

Jan 1, 1924

By E. C. W. Perryman

The recovery of X-ray line broadening, hardness, and electrical resistivity from cold worked AI-Mg alloys has been investigated. The results, together with those from density measurements, suggest that magnesium atoms freeze in the excess vacancies formed by cold working, and that this affects the climb of dislocations during the recovery process. PREVIOUS work1, " has shown that while 1 pct Mg increases the activation energy for recrystalliza-tion, it decreases the activation energy for the recovery of mechanical properties and decreases the subgrain size both after cold working and annealing. A similar result has been reported by Varley2 for an A1-2 pct Mg alloy. With plastic deformation at high temperatures, McLean and Farmer' and Rachinger have found that magnesium appears to retard the motion of dislocations and, furthermore, they find little or no effect of magnesium on the size of subgrains formed during high temperature deformation. In view of the apparent contradictions as to the effect of magnesium on subgrain size, the recovery process in Al-Mg alloys has been investigated more thoroughly by studying the annealing out of X-ray line broadening, hardness, and electrical resistivity from alloys cold worked at room temperature. Material Used—The chemical analyses of the alloys are given in Table I. Fabrication—The material used was cold rolled 20 pct at room temperature, the grain size prior to the last cold rolling operation being similar to that used in previous work; i.e., 230. The experimental procedure for annealing, determination of X-rav half-veak breadth. hardness measurement, electEica1 resistivity, and density and metallographic examination was exactly the same as previously described." Variation of X-Ray Half-Peak Breadth with Annealing Time—Isothermal annealing curves at 100°, 200°, and 250°C were obtained for material cold worked 20 pct. The half-peak breadth of the (333) Ka, line directly after cold working is shown as a function of magnesium content in Fig. 1. Only with the 2.87 pct Mg alloy was overlapping of the a, and n.. reflections observed to any appreciable extent. To separate these, Rachinger's method' was used. Typical isothermal annealing curves are shown in Figs. 2 and 3 for 100" and 200°C, respectively. These curves are similar to those obtained previously for super-purity aluminum except that the

Jan 1, 1957

By Herbert Kynor

BY THE term mechanical mining is meant that operation, or series of operations, that replace the hand methods of mining. The first undercutting machine to operate in anthracite was placed in the Butler mine of the Hillside Coal & Iron Co., Dec. 23, 1910, by the Sullivan Machinery Co. The first Jackhamer used in the anthracite field was installed at the Wadesville colliery of the Philadelphia & Reading Coal & Iron Co. in Oct., 1912, by the Ingersoll-Rand Co. The first longwall conveyor was installed at the Dodge mines of the Delaware, Lackawanna, & Western Coal Co. in March, 1912. The first mechanical scraper equipment was installed in the Seneca mines of the Lehigh Valley Coal Co. in January, 1914. The amount of anthracite mechanically mined since the first mining machine was installed in 1910a is as follows: PENNA. COAL Co. D. L. & W., SCRANTON TEMPLE HUDSON YEAR AND HILL- TONS COAL Co., COAL CO., COAL CO., TOTAL. SIDE COAL TONS TONS TONS TONS AND IRON, TONS 1920 372,737b 367,000d 322,892 74,127 371,878 1,508,634 1919 950,786 no record 306,616 81,575 319,356 1,658,333c 1918 917,778 744,966 24,880 44,756 288,781 2,021,161 1917 757,940 838,800 5,050 57,279 164,180 1,823,249 1916 286,780 860,663 13,960 114,173 101,475 1,377,051 1915 428,819 592,169 8,253 1,029,241 1914 219,188 153,896 373,084 1913 171,505 171,505 1912 124,267 124,267 1911 40,319 40,319 1910 1,184 1,184 a. A slightly greater production than shown was obtained as the tonnage from individual operations is not shown. b. Decrease due to strike conditions in 1920. c. Does not include tonnage of D., L., & W. d. D., L., & W. decrease in 1920 due to having less mining machines in operation. There are about 150 undercutters in use in the anthracite region, 80 mechanical loaders, and 10 longwall conveyors.

Jan 9, 1921

By G. Willard Quick, John R. Freeman

Jan 1, 1930

By Robert M. Grogan, Gill Montgomery

Fluorspar, the commercial name for fluorite, is a mineral composed of calcium fluoride, CaF,. Its valuable properties are due to its content of fluorine, and it is the principal commercial source of that element. The name is derived from the Latin word "fluere," to flow, because the mineral has a low melting point and is used in metallurgy as a flux. Cryolite is a sodium aluminum fluoride, Na,AlF,. It is a rare mineral which has been found in commercial quantities in only one place in the world, Greenland. Small amounts of it are shipped from stock in that country, and its place in industry has been taken over almost completely by synthetic cryolite. Because of the relative unimportance of cryolite, discussion of it has been relegated to a short section at the end of this chapter, which is principally concerned with fluorspar. History Fluorspar was used for ornamental purposes by the Greeks and Romans, who fashioned such things as vases, drinking cups, and table tops from it. Various peoples including the Chinese and the American Indians carved ornaments and figurines from large crystals. Its usefulness as a flux was known to Agricola (1564), who wrote about it in 1546. Mining began in England about 1775 and at various places in the United States during the period 1820 to 1840. Production became substantial following the development and widespread adoption of the basic open hearth method of making steel, in which fluorspar is used as a flux. After that, production and usage were stimulated by growth in the steel, aluminum, chemical, and ceramic industries and were accelerated by World Wars I and II. Fluorocarbons entered the picture in 193 1 and the use of anhydrous hydrogen fluoride (HF) as a catalyst in the manufacture of alkylate for high octane fuel blends began in 1942. The development of the froth flotation process in the late 1920s, a differential flotation scheme for separating fluorspar from galena, sphalerite, and common gangue minerals in the 1930s, and the application of heavy-media concentrating methods to the treatment of low grade ores in the 1940s were outstanding technological contributions that enabled increased production of fluorspar concentrates. In recent years the development of pelletizing and briquetting processes for making flotation concentrates into gravel-size particles for use in steel furnaces and the development of more efficient and selective flotation schemes for treating crude ores containing abundant dolomite and barite have been major improvements in the industry.

Jan 1, 1975

By S. E. Bronisz, Dana L. Douglass

a Uranium was deformed by cold rolling, and the effects of this plustic deformation on the microstruc-ture of the metal were observed by the technique of transmission elecbon microscopy. The recrystalli-zation of selected cold-wmked samples was also studied by this method. The samples were prepared for examination by electrolytic thinning in a standard metallographic electrolyte which has not been previously reported as being used in producing thin foils of uranium. The microstructural changes observed in the a uranium were generally similar to those seen by optical microscopy. The changes in the microstructure of a uranium following cold work and recrystallization treatments have been the subjects of several studies employing optical and X-ray techniques.12-19 These studies indicated that twinning was the redominant mode of deformation at room temperature20 and that the regions of high energy associated with the deformation twins were preferred sites for the initiation of recrystallization.15,18, Recently several workers have prepared thin foils of uranium suitable for examination by transmission electron microscopy.'-lo The foils thus prepared have been used to study fission fragment damage; a particular dislocation reaction,' and gas precipitation." At this laboratory the microstructural changes occurring during the cold working and recrystallizing of a uranium samples have been studied by using transmission electron-microscopy techniques. The foils used in this work were electrolytically thinned in a polishing bath not reported previously in the literature as being used for this purpose. EXPERIMENTAL PROCEDURE The uranium used in this investigation was depleted a uranium sheet 4 mils thick. The results of a spectrochemical analysis of this material are shown in Table I. The as-received uranium was cut into strips, 1 in. wide by 5 in. long, and annealed in vacuo at 600°C for 2-1/2 hr. The resulting microstructure consisted of relatively uniform, equiaxed grains having diameters of 10 to 50 p. Cold Working. The cold-worked samples were prepared by rolling several of the annealed uranium strips to various thicknesses. The strips were reduced 3.5 ± 0.5, 6.0 ± 0.6, 10.0 ± 0.5, 19.5 ± 1.0, and 28.5 ± 2.0 pct in thickness. It was not possible to achieve these reductions with a single pass through the rolling mill, so the strips were turned end for end during the rolling procedure. The cold-rolled strips were stored in dry ice until samples from them could be thinned and examined (within 24 hr after rolling). Annealing. The samples used in studying the re-crystallization behavior of a uranium were obtained by annealing sections of the strips which had been reduced 10.0 and 28.5 pct. These samples were sealed in evacuated Pyrex capsules and were annealed in a tube furnace at temperatures from 200" to 600°C and for times from 1/2 to 2 hr, see Table l. Thinning: The samples from the rolling and heat treatments were prepared for examination in the electron microscope by electropolishing in a bath composed of 25 g chromic acid, 133 ml glacial acetic acid, and 25 ml water. This electrolyte has been used and recommended for preparing specimens for optical metallography It was necessary to mask the edges of the sample with a stop-off paint in order to prevent preferential attack in these areas. The paint used was made by dissolving polystyrene in benzene. The electrolytic cell consisted of a cylindrical stainless-steel cathode placed in a beaker containing the electrolyte, with the sample as the anode positioned at the cell axis. The temperature of the electrolyte was held below 15°C by cooling with liquid

Jan 1, 1963

Jan 1, 1934

By Earl S. Bardwell

The determination of suitable and safe annealing temperatures is one of the most important problems arising in the operation of a copper rolling mill. Certain of the larger mills have worked this problem out for themselves and in these mills the operation has become more or less standardized. In some of the mills pyrometers are used to measure the temperature of the annealing furnaces and careful watch is kept to see that overheating does not take place. In a considerable number of the mills, however, dependence is placed entirely on the judgment of the operator. The almost total lack of literature bearing on this subject seems sufficient warrant for the publication of this paper. ' The discussion of this subject naturally divides itself into two parts: (1) The effect of annealing temperature on physical properties; and (2) changes in the microstructure of refined copper due to cold rolling and annealing. I. The Effect of Annealing Temperature on Physical Properties For the purpose of investigating this phase of the subject six test bars were selected, varying in oxygen content between the limits of 0.036 and 0.070 per cent. The chemical composition of each of these test bars was as follows: Bar Number 1 2 3 4 5 6 Copper + silver...... 99.95 99.92 99.945 99.94 99.95 99.93 Oxygen.............. 0.041 0.070 0.046 0.050 0.036 0.058 As + Sb............. 0.0038 0.0038 0.0038 0.0038 0.0031 0.0031 The bars were heated in an electric muffle to about 1,650" F. and rolled into rods. The rods were annealed, pickled, and drawn to No. 12 B. & S. gauge wire. The wire which was to be used for the annealing test was cut into 38-in. lengths and each length made into a coil 6 in. in diameter. The separate coils were marked so that they might readily be identified

Jan 1, 1915