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By George L. Heath

It may at first appear doubtful that any further ideas can now come from such a well-trodden soil, when we consider that the ground of the subject has been so thoroughly gone over in many of its phases and that observations have been recorded in technical journals, ever since the days when Luckow and his cotemporaries brought the electrolytic deposition of pure copper to the position of an exact scientific method. Certain facts, however, which seem worthy of note, have come under the writer's observation during an extended use of the method in a large refinery, involving frequent tests of refined Lake and electrolytic copper, and thousands of assays of native copper concentrates and tailings. This work has required a careful study of the conditions suited to the assay of refined copper, and of ores and tailings— conditions which must be varied for each particular case to secure the best results. Especially is this true when we come to the exact determination of pure copper in the high-grade refined metal of the present day. Very slight traces of impurities (especially tellurium, selenium, bismuth, tin, arsenic and antimony) seriously injure the properties of copper, notably its electrical conductivity. The increasing demands of electrical science and construction lead to the conclusion that the analysis of all high-grade American coppers, at least, has become, and must be in future (in or-

Jan 1, 1898

By L. L. Wyman

PREVIOUS studies1 by the writer dealing with the embrittlement of copper have been concerned with the behavior of various pure and deoxidized coppers when exposed to an oxidation-reduction cycle, and the consequent evaluation of these materials on the basis of their resist-ance to this action. No attention was devoted to the variations in pene-tration of embrittlement with time, when these copper materials are exposed to a strong reducing gas, such as hydrogen, nor to the variations in oxygen penetration, with time and temperature, into the "pure" coppers. The cause of the embrittlement is the reduction of the oxygen in the copper by the hot reducing gas, so that a consideration of time, tempera-ture, the occurrence of hydrogen and oxygen must be given. For the purpose of differentiating some of "the involved factors, the present work may be divided into two separate series of experiments. The first of these deals with the oxidation of purified coppers under various conditions and then the subjection of these to a standard hydrogen treatment. The second series concerns the reduction, under different conditions, of tough-pitch coppers of several oxygen contents. The resulting data will give the rates of oxidation, and of reduction, for the materials involved. The first series of experiments will reveal how rapidly copper may become oxidized, while the second series will indicate how rapidly embrittlement will penetrate into an oxygen-containing copper when it is exposed to hydrogen at different temperatures.

Jan 1, 1933

By M. Paulus

It is known that multicomponent powders are mostly nonhomogeneous. This paper investigates the effects of nonhomogeneity of composition and grain size on the melting point and the sinterability of compact taking into account homogenization mass transport and the length of the diffusion path in solid state sintering, and the kinetics of liquid phase formation in liquid phase sintering. After a discussion on the ideal characteristics of a powder for sintering and low temperature reaction, the main conventional processes are compared. Finally we develop the freeze-drying technique and demonstrate the capabilities and the limits of the process by some examples, mainly in the ceramics field.

Jan 1, 1980

By R. W. Nelson

Methods for determining permeability presented by W. D. Kruger3 in a paper entitled "Determining Areal Permeability Distribution by Calculation" have considerable merit. They can be expected to contribute significantly to analysis of flow in heterogeneous systems. Some rather subtle yet important conditions must be met, however, to assure that the computed permeabilities are correct. The conditions which insure a unique permeability distribution may have been overlooked in the method as proposed and presented in the subject paper. The subtlety of the special requirements may permit good agreement between computed and measured pressures in the reservoir; but the computed permeability may still be in error. The general theory and discussion of the requirements for a unique determination of the permeability distribution are presented elsewhere in more detail.7'8 Accordingly, only major features will be presented here in the notation of Kruger. GENERAL DESCRIPTION OF REQUIREMENTS A brief mention of the route to be followed in showing the special requirements may be helpful. The equation to be solved is a quasilinear, first-order, partial differential equation in the unknown permeability. This equation can be solved through an extension of Lagrange's method by reduction to a system of subsidiary ordinary differential equations. Through consideration of the identity of one of the Lagrange subsidiary differential equations with the stream function, a special interrelationship can be shown. The interrelationship has special significance with respect to the boundary condition. If the boundary function satisfies part of the subsidiary differential equation, no unique solution for the permeability distribution exists. In the physical problem this requirement for uniqueness indicates that the permeability measurements used as a boundary condition can not be along a stream tube. The boundary condition must be along a line, or series of lines, which completely traverse the region and pass through every stream tube.

By William White

History.—The making of iron and steel from the ores of northern Mexico was for years a favorite project of the late Don Patricio Milmo, upon whose estate large deposits of coal and iron were known to exist, and with whom Mr. Eugene Kelly, of New York, was associated. Several expert examinations of the property mere made for them; and when failing health forced Sr. Milmo to retire from active part in the matter, Mr. Kelly carried on the project and associated himself with Messrs. Vicente Ferrara, of Monterrey, Antonio Basagoiti and Leon Signoret, of the City of Mexico, and other leading citizens of Mexico, Monterrey and New York, who, in May, 1900, organized the " Compania Fundidora de Fierro y Acero de Monterrey," with a capital of $10,000,000. The main reason for locating the plant at Monterrey was, that a circle drawn with Monterrey as a center, and the distance from Monterrey to Laredo as a radius, will contain all the known Deposits of iron-ore of Bessemer quality, and the greater part of the available coal, in the Republic. Moreover, Monterrey is connected with all the Mexican trunk railwaylines, and thus with the Gulf of Mexico, and supplies, therefore, the conditions necessary for prosperous manufacturing, namely, cheapness in assembling raw materials and means for wide distribution of product. It also has a number of enterprising citizens, who have been successful in mining, smelting and manufacturing operations, and a sufficiently large population to supply the necessary labor. Iron-Ore.—The company's iron-mines are on the Carrizal mountain, on the Mexican National, and at Monclova, on the Mexican International railroad. At the former locality, two mines, Piedra Iman and the Anillo de Hierro, sufficiently large

Jan 1, 1902

By S. R. B. Cooke, C. E. Thurston, G. Kudo

The trend toward utilization of low grade iron ores means that more efficient methods must be developed for their concentration. The collecting ability of fatty acids derived from fish oils has been extensively investigated by Cooke.' Tuna oil, a byproduct of the tuna canning industry, is one of the lower priced fish oils. Utilization of tuna oil fatty acids as collectors in the flotation of iron ore might be economically feasible under certain market conditions, especially if their efficiency were high. Crude or unfractionated tuna oil fatty acids, and five fractions derived therefrom, were tested for their ability to concentrate a commercial specularite ore from northern Michigan. A commercial fatty acid derived from tall oil, and commonly used in nonsulfide flotation, was used as a reference. The crude fatty acids were obtained by simple saponification of tuna oil. Fractions A and B were obtained by acetone precipitation of the crude acids at -5O and -2S°C, respectively. Fraction C was obtained by a partial fractional distillation at 12S°C and at a pressure of 3y in a centrifugal molecular still in order to remove the shortest and longest chain fatty acids of tuna oil as well as oxidation products present in the original mixture. Fractions D and E were prepared by a chilling process in order to precipitate the unwanted saturated fatty acids. Yields and iodine values of the materials used are listed below: The seven samples were used as collectors in a laboratory procedure patterned after the commercial process for flotation of Michigan specularite ore. The outline of the procedure is that previously described1

Jan 1, 1962

By I. N. Zavarine

THE present paper is a continuation of the work on the relationship between the magnetic and the phase transformations in carbon steels during quenching. An account was given by the author in a previous paper1 of an investigation of this relationship during a continuous quench. The experimental difficulties then encountered prevented a conclusive proof of the existence or absence of such a relationship. The conclusions of the previous paper were derived indirectly. The present paper deals with the same problem, but the method of attack is modified. The technique developed by Davenport and Bain2 in their well-known study of austenite transformation at subcritical temperature was adopted in the present investigation.. They have shown that the austenite to martensite transformation can be caused to proceed at a relatively slow rate by quenching steels into a hot metal bath. Slowing down of the rate of transformation, together with an observation by Lewis3 that a eutectoid steel can be preserved in the nonmagnetic state by such quenching, pointed out a possibility of a study of both transformations .under more favorable conditions than previously described. The preliminary steps were connected with the technique of the hot bath quench. To study this phase of the present work a modification of the apparatus previously described1 was used. The modification consisted in the use of a hot quenching bath instead of brine, and in fixing the secondary and the primary coils of the apparatus in a stationary position in and around the bath. Tubular specimens, as in the previous investigation, were heated in a suitable furnace to a temperature in the austenitic

Jan 1, 1935

By Helmer Hedstrom

THE purpose of this paper is to direct attention to the importance and the usefulness of phase measurements in electrical prospecting for ore, a subject about which virtually nothing has been published. The paper describes a new field method for ore prospecting, the "Turam" method, which makes use of phase measurements, and which has been used with great success for five years. Of the principal geophysical prospecting methods, the gravimetric and magnetic methods determine the direction and strength of the static fields of force of the earth. By seismic and electrical methods, fields of force are applied to the block of ground under investigation. By these methods a third parameter can be measured, besides the direction and strength of the field; namely, the time of arrival of the applied field at the different observation points. This time of arrival has been practically the only parameter measured in seismic work, while in electrical pros-pecting it has generally not been considered, the measurements having been limited to determination of direction and strength of the applied field.

Jan 1, 1937

By A. Boltax

The effect of cold work on the electrical and magnetic properties of solution-treated and aged Cu-Fe alloys was studied. The electrical resistivity of solution-treated and of aged Cu-1.7 wt pct Fe samples increased by up to 25 and 140 pct, respectively, follozcing a 55 pct reduction of area. The principle contributions to the increase of resistivity of the solution-treated and aged samfiles are examined. Measurements of the .saturation induction, coercive force, and stacking fault Probability are also reported. 1 HIS paper is the second in a series which examine the behavior of the electrical and magnetic prop- erties of Cu-Fe alloys. The first paper1 was primarily concerned with the effects of thermal treatment whereas the present paper examines the effects of cold work on solution-treated and aged Cu-Fe alloys. The effects of cold work on the transformation of the coherent fcc iron precipitate to the ferromagnetic form2 and the coercive force and remanence3 have already been described, but the unusually large increases in resistivity (up to 220 pct) which occlir with cold work have not been reported previously. EXPERIMENTAL METHOD The methods used for alloy preparation, heat treatment, and electrical and magnetic measurements are described elsewhere.1 The specimens, initially 4-in. lengths of 0.0625-in. diam wire, were cold worked by swaging in hardened steel dies. Following each reduction, the samples were etched lightly in hydrochloric acid to remove surface con-

Jan 1, 1962

By J. B. Hess, C. S. Barrett

TO reach equilibrium between different phases in cobalt-rich alloys requires prohibitively long annealing cobalt-richalloystimes when temperatures are below about 700°C. The fact that a transformation from face-centered cubic to close-packed hexagonal readily tered takes place at temperatures below this in the cobalt-rich solid solutions is not an indication that thermally activated processes occur at an appreciable rate, for the transformation is well established as martensitic in nature. Wide divergence between heating and cooling experiments and high sensitivity to prior heat treatment make it difficult to judge temperatures of equilibrium between the phases.&apos; One object of the present work was to see if the information object of on the relative stability of phases could be gained by substituting plastic deformation for thermal agitation. Procedures were worked out that led to the determination of a diffusionless type of phase diagram, which represents the temperature of of phase equal stability for phases of the same composition, and the technique was applied to the Co-Ni system. Another object of the work was to see whether or not deformation would generate frequent stacking faults when these were thin lamellae of quentstackingfaultsa phase having higher free energy than the parent phase. The alloys were prepared in 80 to 100 g melts from cobalt (with metallic impurities estimated spectrochemically as follows: Ni, 0.05 pct; Fe, 0.001 pct.; Mg, Si, Cu, Cr, Al, < 0.001 pct) and Mond Car-bony1 nickel (with Fe, 0.05 pct; Si, 0.003 pct; C, 0.61 pct.; Cu, 0.001 pct; Co, Cr not detected, < 0.01 pct). The metals were melted in pure Al2O3 crucibles. An atmosphere of argon, that had been purified by passing over hot magnesium chips, was used for the alloys that, by analysis of the portions of the ingots actually used, were found to contain 15.3, 25.7, and 35.0 pct Ni, and vacuum melting (after degassing) was used for those containing 29.4 and 31.5 pct Ni. After induction melting the alloys were allowed to solidify in the crucible, and slices % in. thick x ½ in. in diam were annealed 12 hr at 1350°C for homogenization. These same specimens were used throughout the series of experiments, with annealing treatments of 4 hr at 900°C in purified hydrogen followed by furnace cooling, alternating with the deformation and X-ray tests discussed below. Results Spontaneous transformation was observed on cooling to room temperature in all alloys containing 29.4 pct Ni or less and by cooling the 31.5 pct alloy to — 195°C but was not observed in the 35 pct alloys after cooling to —195°C. These results are in satisfactory agreement with the cooling experiments of Masimoto.4 From these data it is clear that the temperature of beginning transformation M,,, drops to 20°C with the addition of about 30 pct Ni. The test for spontaneous transformation was metallographic. Specimens were thermally polished by annealing 10 hr in hydrogen at 1350°C, then furnace cooled; if trans- formation had occurred there were relief effects visible on the thermally polished surfaces. These markings were narrow straight lines, usually resolvable at high magnification as clusters of fine lines that resembled slip lines. It was concluded that they resulted from displacements on (111) planes, for the number of directions in individual grains often reached but never exceeded four, and lines could always be found parallel to the thermally etched (111) boundaries of annealing twins. The markings were thus consistent with the idea that the transformation occurs by (111) plane displacements (Shockley partial dislocations moving on (111) planes). This was further confirmed by X-ray tests for stacking disorders. Using an oscillating crystal technique previously employed to detect strain-induced faulting in Cu-Si alloys," streaks indicative of the stacking faults were looked for and found on X-ray films of the spontaneously transformed 25.7 pct Ni alloys, as expected by analogy with Edwards and Lipson&apos;s results on pure cobalt." The streaks were much intensified after rolling at room temperature. Transformation induced by plastic strain was investigated as a function of alloy composition and temperature of deformation. A series of tests was made to determine suitable straining and X-raying techniques. Filing was found inferior to abrasion in converting cubic samples to hexagonal, and abrasion was less effective than peening in producing smooth unspotty Debye rings in the X-ray patterns. Because the diffraction lines were broad, Geiger-counter spectrometer records of filings were less sensitive in revealing small amounts of transformed material than X-ray patterns recorded on films in a small diameter camera. After these exploratory tests the following methods were adopted. Specimens that had been annealed at least 4 hr at 900°C and furnace cooled were mounted in a block of aluminum, brought to temperature, and peened thoroughly with a mullite pestle preheated to the same temperature. The specimens were then quenched to room temperature. In peening, a circular area of % in. diam was given 500 blows. A few control tests showed that an additional 1000 blows did not detectably change the proportions of the phases present. The amount of transformation was judged by X-ray reflection patterns from the peened surface, using the innermost four lines of the cubic and the hexagonal patterns with filtered CoKa radiation,

Jan 1, 1953

By A. R. Denison

This field in 1933 continued as in 1932, although to a much less extent, to dominate the drilling and production situation throughout the oil business. The 2466 producers completed in this field during the year are 28 per cent of such wells completed in the United States. The 2556 completions reported in the five counties within which the East Texas field lies are 21 per cent of all such wells reported in the United States. It follows that with such a command of the development situation, every other factor with regard to this field has an important bearing on the entire oil business. As a consequence, the important developments in the East Texas field are the important developments of the year. Very little new productive territory was added to the already known limits of this enormous field. On the other hand, drilling has shown that with a few very minor exceptions this field is a continuous productive area, with a regular outline and no "dry spots" other than that of a single well surrounded by producing wells. Drilling was confined to the already proven limits of the field. This consisted essentially of more adequate coverage of leases by wells, the meeting of required offsets and the drilling of a large number of small tracts which developed from subdivision of larger leases due to court action and other causes. The allowable throughout the year was, with minor variable factors, on a per-well basis. With the steady decline in per-well allowable after May, every operator was faced with declining

Jan 1, 1934

By Robert E. Green, Wolfgang Sachse

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

Jan 1, 1969

By Frank L. Nason

In the year 1904 an eminent Swedish geologist prepared a report on the iron-ore reserves of the world. His estimates follow: Countries. Tons. United States,.1,100,000,000 Great Britain,.1,000,000,000 Germany,.2,200,000,000 Spain,.. 500,000,000 Russia and Finland,...... 1,500,000,000 France,..1,500,000,000 Sweden,..1,000,000,000 Austria-Hungary,....... 1,000,000,000 Other countries,1,200,000,000 Total,.10,000,000,000 The iron-ore allotted to the United States by the Swedish geologist is barely sufficient to last 20 years at. the present rate of consumption. On the other hand (according to Edwin C. Eckel,&apos; from whom the above and following statistics are quoted), there is hardly need for worry on the part of our iron industries for the next two centuries or more. Upon the basis of careful work by the U. S. Geological Survey, in which Mr. Eckel has taken an important part, the following estimates are definitely, but by no means finally, given for the United States: District. Tons. Lake Superior District,... 1,500,000,000 to 2,000,000,000 f red hematite,.. 1,000,000,000 Alabama, brown hematite, hematite, . 725,000,000 red hematite,.. 200,000,000 Georgia, { brown hematite, . 125,000,000 Tennessee, { red hematite,.. 600,000,000 Tennessee, { brown hematite,hematite, . 225,000,000 f red hematite,.. 50,000,000 Virginia, } brown hematite, . 300,000,000 Total,..4,725,000,000 to 5,225,000,000

Jan 1, 1913

By Robert C. Berggan

The hot-milling process for reconditioning rock-drill bits is not new. It has been employed by a few mines for years and in the past decade it has been widely adopted, as its advantages have become better known. Because of the extensive commercial development in England and Canada of machines to operate on this principle, general acceptance has been largely in the British possessions and until recently has been chiefly in the field of conventional steel. In the past two years there has been a definite trend toward hot-milling of detachable bits in Canada, but only in the past year has any considerable attempt been made to build special machines for this type of work. Generally a machine designed for conventional steel has been used and special holders employed to manipulate the bit. As early as 1934 at least one operator in the United States had adapted hot-milling to conventional steel with a substantial saving in resharpening costs.1 Several other operators have taken it up but there has been no widespread adoption of the method in this country by users of conventional steel. This may be partly explained by the fact that until recently no American manufacturer produced this equipment and operators have been obliged to build their own hot-millers or import them. Several years ago a few machines were built in Seattle, Washington, and operated in some mines in the northwest, but, for reasons not generally known, the effort was abandoned. The Process Hot-milling performs the function of re-dressing the bit at a forging temperature of about 1650°F., by the removal of metal from the flutes with a milling cutter, followed by a similar cut from the bit gauge. Conventional bits are thus treated following the usual forging operation in a sharpener, and usually in the same heat.

Jan 1, 1940

By Robert C. Berggan

The hot-milling process for reconditioning rock-drill bits is not new. It has been employed by a few mines for years and in the past decade it has been widely adopted, as its advantages have become better known. Because of the extensive commercial development in England and Canada of machines to operate on this principle, general acceptance has been largely in the British possessions and until recently has been chiefly in the field of conventional steel. In the past two years there has been a definite trend toward hot-milling of detachable bits in Canada, but only in the past year has any considerable attempt been made to build special machines for this type of work. Generally a machine designed for conventional steel has been used and special holders employed to manipulate the bit. As early as 1934 at least one operator in the United States had adapted hot-milling to conventional steel with a substantial saving in resharpening costs.1 Several other operators have taken it up but there has been no widespread adoption of the method in this country by users of conventional steel. This may be partly explained by the fact that until recently no American manufacturer produced this equipment and operators have been obliged to build their own hot-millers or import them. Several years ago a few machines were built in Seattle, Washington, and operated in some mines in the northwest, but, for reasons not generally known, the effort was abandoned. The Process Hot-milling performs the function of re-dressing the bit at a forging temperature of about 1650°F., by the removal of metal from the flutes with a milling cutter, followed by a similar cut from the bit gauge. Conventional bits are thus treated following the usual forging operation in a sharpener, and usually in the same heat.

Jan 1, 1940

By F. F. Aplan

INTRODUCTION Coal is a solid combustible mineral substance resulting from the alteration of vegetable matter largely in the absence of air. It occurs in nature with varying percentages of mineral matter associated with and incorporated into the coalified material. If the amount of this inorganic mineral matter is sufficiently small, and if selective mining can be practiced so as to avoid the incorporation of ash- bearing material from adjacent strata and/or parting seams, the coal can be used as-mined. Otherwise, it must be given a preparation treatment. In 1980 the bulk of the approximately 525 coal preparation plants were located in the eastern half of the U.S., largely in the Appalachian and to a lesser extent in the midwest coal fields (1). Only 17 of these preparation plants were located in the west; these were in Colorado, New Mexico, Utah, Washington and Wyoming. In the past, however, a great many more preparation plants were operated in these and other western states. The upsurge in both the domestic and world- wide demand for quality coking and steam coal will certainly lead to an increase in the number of preparation plants in the west. In fact, there has been a massive development of coal mines and their associated preparation plants across our northern border in Alberta and British Columbia, largely to serve the export coking and steam coal market. Most of the tremendous increase in newly-mined coal in the western U.S. has come from thick seams of inherently low-sulfur, low- ash coal, easy to mine selectively without significant contamination with ash-forming minerals and requiring no preparation. Because of

Jan 1, 1983

By G. A. Chadwick, D. Jaffrey

The morpho1ogies and orientation relationships of the phases in the Sn-Zn and A1-A13Ni eutectic systems were examined by electron microscopy and X-ray diffraction techniques. In each alloy the "transition" from the lamellar to the fibrous morphology was found to be one of scale, not of type. The minor phase in both systems exhibited certain well developed facets which were not affected by changes in the ingot solidification rate. The crystallographic relationships displayed by the pairs of phases in both systems were also insensitive to the growth rate. In the Sn-Zn alloy, the unique relationship of: growth direction - II [1201 Sn - II [01101 Zn and ribbon interface plane 11 (101) Sn 11 (7012) Zn was determined. The Al-Al3Ni alloy phases did not possess any particular orientation relationship, though the Al3Ni phase invariably grew in the [010] direction and exhibited the same set of facet planes. These results are discussed in relation to current eutectic growth theories and explanations of the "lamellar to fibrous transition". THE lamellar to fibrous transition that occurs in many eutectic alloys has been the subject of considerable speculation and experimental study. In some alloys it can be induced solely by an increase in the solidification rate,&apos;-3 whereas in others the transition supposedly occurs only if the lamellae are forced to grow out of the overall ingot growth direction.4-6 he cause of this latter type of transition has been attributed to deviations of the lamellae from their low energy habit planes;4&apos;5&apos;7 fibers are produced because the sustaining force for lamellar growth (a low energy boundary) is destroyed. Implicit in these explanations is the assumption that fibers are circular in cross-section and completely lacking in low energy inter-phase interfaces. The "natural" growth rate dependent transition has been studied less thoroughly although Tiller8 has attempted a theoretical explanation of it. Tiller&apos;s arguments are not completely satisfactory9 but his suggestion that the relative undercoolings of the solid/liquid interface for lamellar and fibrous morphologies are growth rate dependent cannot be totally discounted; it is possible, for instance, that the relative interfacial undercoolings could alter and produce the observed morphology change if the orientation relationships between the phases and the associated interphase bound- ary energies were sensitive to growth rate. Salkind et al." have reported finding a change in the orientation relationships in the A1-A13Ni system accompanying the lamellar to fibrous transition, but contradictory evidence has also been reported for this3&apos;" and another system,12 so the position remains unclear. In an attempt to clarify matters a study was made of the "lamellar to fibrous" transition in the Sn-Zn and A1-A13Ni eutectic systems; the morphologies of these two selected systems are quite similar when viewed by optical microscopy. In the present research the morphologies and morphology changes were investigated by electron microscopy. The orientation relationships existing between the eutectic phases were also determined for both morphologies in both eutectic systems. EXPERIMENTAL PROCEDURE The materials and method of alloy preparation and ingot solidification for the Sn-Zn system have been reported previously.2 In this investigation nine horizontally grown ingots of the highest purity (99.9997 pct) were used. The temperature gradient in the melt was not intentionally varied and was approximately 10°C per cm. Seven growth rates between 1.3 cm per hr and 20 cm per hr were imposed. The A1-A13Ni alloys were prepared from "Spec. Pure" nickel and 99.995 pct aluminum by melting the components in an open alumina crucible and casting the melt into the cold graphite mold. Six ingots of the Al-Al3Ni alloy were unidirectionally solidified at growth rates from 1 cm per hr to 12 cm per hr under high purity argon. A typical ingot was 20 cm long, 1 cm wide, and 0.75 cm to 1.5 cm thick. Samples taken from the bars at positions 12 cm from the nucleation end were examined by conventional orthogonal-section metallo-graphic techniques. When required, samples were mounted for X-ray diffraction analysis using the Laue back-reflection technique with a finely focussed X-ray source. The surfaces of the A1-A13Ni specimens were prepared by mechanically polishing them down to the 1 µ diamond pad stage followed by an electropolish in 80/20 methanol/perchloric acid solution at 0°C and 20 to 30 v. The Sn-Zn specimens were repeatedly polished on an alumina pad and etched in hot dilute (2 pct) nitric acid until the diffraction spots were found to be sharp. Thin films of the alloys were prepared for observation in an electron microscope by spark machining thin discs (0.03 to 0.04 in. thick) from longitudinal and lateral sections of the bars and elec-trolytically thinning them via a jet polishing technique. For the A1-A13Ni eutectic alloy, an 80/20 mixture of ethanol/perchloric acid at 40 v and 20°C was found to be satisfactory. A solution of 70/20/10 methanol/perchloric acid/butylcellosolve at 25 v and 20°C was used on the Sn-Zn alloy. For the former alloy the jet nozzles (cathodes) and the disc clamps were of aluminum;

Jan 1, 1970

By P. W. Gilles, B. D. Pollock

THE pioneering work of Steinitz1 and Steinitz, Binder, and Moskowitz2 has shown conclusively the existence at high temperature of two additional phases in the molybdenum-boron system and thus brings to a total of six the number of structures appearing in this system. To the structures Mo2B, MOB, and Mo2B5 they have added MO3B2, a new -MOB form, and have shown that MOB,, which has the same range of composition as Mo2B5, is only a high temperature structure of the latter. This solid solution, interestingly enough, includes neither of the compositions corresponding to the stoichiomet-ric compounds, MOB, or Mo2B5, but rather at all temperatures has intermediate values of composition. These workers have also, in the course of their work, measured melting points, transition temperatures, eutectic and peritectic points in the system and have shown that Mo3B2, because of its dispro-portionation at low temperature to Mo2B and MOB, is stable only in a limited high temperature range. During the course of the present work on the vaporization properties of the molybdenum-boron compounds, a few transition temperatures were observed. When the report of the other workers appeared, it was decided to repeat, in part, their study of the system. As a result, considerable evidence has been obtained that substantiates the specific kinds of melting processes they report as well as the general features of their diagram. However, a marked difference was found between the temperatures they report and the ones observed in this study, with the latter being higher. The purposes of this paper are to present the evidence obtained in this laboratory that verifies their diagram of the system, to give some important temperatures in the system, to compare them with those previously published, and to seek an explanation of the difference. Samples The metal starting material was 400 mesh molybdenum powder with a purity stated by the manufacturer to be 99.9 pct. The initial treatment, designed to remove volatile contamination, consisted of heating in a vacuum for 10 min to a temperature of from 800" to 1000°C during which a loss of 0.3 to 0.4 pct occurred. An assay following this treatment showed it to be 99.4 pct pure, with the principal impurity probably being oxygen. The boron starting material was obtained from the Cooper Metallurgical Laboratories and the Fair-mount Chemical Co. as 325 mesh powder with manufacturers&apos; analyses of 99 pct or better. Initial treatment consisted of heating in molybdenum in a vacuum at about 1700°C for 10 min. During this time a loss of 3.5 pct occurred. An assay following this treatment showed the different samples to have purities ranging from 95.5 to 99.0 pct with iron and carbon as the principal impurities. Following the initial treatment, the elements were combined to form stocks of Mo2B and MOB by heating pressed mixtures in a vacuum to 1100" to 1200°C to accomplish reaction and to 1500" to 1900°C for a few minutes to evaporate the more volatile impurities. Analysis of the two compounds for boron by a modification of the method of Blumenthal3 and for molybdenum by the lead-molybdate method indicated them to have purities greater than 99 pct. The individual samples to be studied had compositions in the Mo2B-MOB range and consisted of mixtures of the stock compounds. Procedure As is usually the case in high temperature work the selection of containers for the samples posed some problems. For vapor pressure studies tantalum crucibles, allowing little contact with the pressed samples, were used and some of the observations made during these experiments are pertinent to the study of the phase diagram. Most of the experiments, however, were performed in graphite containers, as were those of the previous authors. Two kinds of spectroscopic grade graphite crucibles were used. One was a % in. cylinder, 3/4 in. high, containing seven 3/16 in. holes drilled 1/2 in. deep into which were packed samples of the different mixtures weighing 250 to 500 milligrams. The other, consisting of separate crucibles, was prepared by drilling 3/16 in. holes, 1/2 in. deep into 1/4 in. graphite rods % in. long. The 7/8 in. cylinder was heated directly by induction while the small crucibles were packed in a tantalum heating element for induction heating. All heating was done in a high vacuum system in which the pressure was generally less than 1x10-5mm and never rose above 2x10-5mm when the samples were hot. The general pattern of the heating in graphite was to heat rapidly to a temperature somewhat below the desired one, then to raise the temperature slowly. The samples were held for 2 to 5 min at the maximum temperature, which in all cases was far higher than that needed to produce reaction. The short time was employed to reduce possible contamination by the crucible material and to reduce composition changes that would occur because of vaporization. After examination following the heating, the samples were reheated to a higher temperature. Temperatures were measured with a Leeds and Northrup disappearing filament optical pyrometer, certified by the National Bureau of Standards, by sighting through a window at the top of the vacuum

Jan 1, 1954

By A. E. Lillstrom

IN the development of iron mines and production of iron ore from the Marquette range, drilling blast-holes is an important phase of the mining cycle. The ground drilled in ore production can be classified into two main categories, soft hematite and hard hematite or magnetite. Within these categories the material exhibits a wide range of penetrability by percussion drills. Development work encounters various types of rock. Slate and altered basic intrusives constitute the softer types commonly encountered. Harder materials are represented mainly by greywacke, quartzite, iron formation, and diorite. Prior to the first tungsten carbide trials in late 1947 and early 1948, hard-rock and ore drilling was done with steel jackbits starting at 21/4-in. diam. These were reconditioned by hot milling. Automatic or handcrank 31/2-in. drifters were employed, mounted on Jumbos, posts and arms, or tripods, depending upon the working place. With the exception of shaft sinking jobs where 55-lb sinker machines were and still are used with 1-in. quarter octagon steel, the other production and development mining utilized 11/4-in. round and Leyner-lugged steel. The following properties have been selected as typical examples wherein carbide bit applications have proved economical. The Mather mine "A" and "B" shafts and Cleveland-Cliffs Iron Co. mines are soft ore mines where insert bits are used in rock development only. The Greenwood mine, Inland Steel Co., Champion mine, North Range Mining Co., and Cliffs shaft mine, Cleveland-Cliffs Iron Co., are hard ore mines where all drilling is done with tungsten carbide bits. Mother Mine "A" Shaft In the Mather mine "A" shaft and other soft ore properties where only rock development work is done with the tungsten carbide bits, several types and makes of bits have been tried since early 1948. The greatest proportion of failures have been at the connection end, although the early trials with the 13 Series Carset 11/2-in. bit used in conjunction with 31/2 -in. automatic-feed drifters, showed an equal amount of shattered inserts. To combat this shattering, the 31/2 -in. drifters were replaced by 3-in. drifters, thus eliminating, for the most part, insert failures. However, the attachment end of the rod continued to be the main source of trouble. The greatest amount of failure was in the stud or at the upset section approximately 2 in. behind the drive shoulder of the rod. Heat treatment was changed several times as well as the composition of the alloy studs. Since this failed to correct the trouble, a decision was made to change to a heavier attachment section. Timken 11/2-in., type M, bits were then employed and showed an exceptional improvement. The rods are discarded when the thread contour shows sharpening or wear on the shoulder. It was also learned that the Timken insert did not show as rapid gage and cutting edge wear as did competitive makes, and footage per use increased by approximately 50 pct. Prior to the Timken trials the average life per bit at the Mather mine "A" shaft on 6-ft change chain-feed drifters was 500 ft, and the rod life at the connection end was 50 ft. The Timken bit with chrome-plated thread averaged 1200 ft, and rod life increased to as much as 500 ft. However, the life of the connection end was much better on shorter length drill rods or in places where machines with 34-in. change were used. The bit thread continued to be the point of ultimate failure with thread strippage, constituting the cause for discard of bits. In one of the new development headings, harder rock was encountered for approximately 800 ft, dropping the life per bit to a low of 90 ft with shank and thread life of rods dropping to approximately 125 ft average. The stripped bits were then welded to the rods, increasing the life per bit by 75 to 100 pct. The rod transportation for main level development was not a problem so intraset rods were tried. Intraset rods have tungsten carbide inserts set into the rods proper by the manufacturer and can be obtained with chisel or four point bits. This type of rod eliminates the need for any connection and the steel being a special alloy will show more feet drilled per rod. The first trial was made with eight rods, and final results averaged 350 ft per rod, six of the rods worked the life of the bit end, and two broke shanks at less than 50 ft. The preceding example showed a considerable improvement, so additional steel of the same type was purchased, but its use has been limited to main level drifting only, because of the handling problem involved in transportation of the complete rod to mine shops for resharpening. Further trials are being made on improving the life per detachable bit by chrome plating. To date, the chrome plating shows an improvement of approximately 100 pct. However, final results will not be known until the present long term trials have been completed. Mother Mine "B" Shaft In November 1947, tungsten carbide bits were first tried at the Mather mine "B" shaft. The use of 1%-in. Carset 13 Series bits, for drilling the 72-hole, 7-ft shaft round, decreased the drilling time from an average of 41/2 hr per round required with steel bits, to 2 hr with insert bits. The best drilling time for

Jan 1, 1952

By Charles M. Packer, Oleg D. Sherby, Roy H. Johnson

Originally round tensile specimens of a eutectic Zn-A1 alloy develop elliptical cross sections during superplastic deformation. This observation, coupled with a detailed study of the microstructure and preferred orieniation, suggests that crystallographic slip and continuous grain boundary migration or re-crystallization are important processes during super-plastic deformation. In spite of the extensive activity in superplasticity1-15 and the numerous explanations proposed, no single model has had universal acceptance. It has been established, however, that the general requirements for superplastic extension of two-phase alloys include an extremely fine, stabilized grain size of the order of a few microns, a temperature about equal to or greater than one-half the melting point, a critical range of strain rate, and a similarity in the mechanical strength of the major phases. The proposed models can perhaps best be characterized in terms of the important phenomena associated with them. These phenomena include: phase instability,1 diffusional creep by volume diffusion3 or grain boundary diffusion4,5 slip and continuous grain boundary migration or recrystalliza-tion,= grain boundary Sliding,7-9,13,14 and dislocation glide.&apos;5 In this paper, experimental observations will be reported which support a model involving slip and continuous grain boundary migration or recrystalliza-tion. Specifically, a correlation will be made between this model and the development of elliptical cross sections as originally round specimens are superplas-tically deformed. For the most part, superplasticity studies have been conducted with eutectic or eutectoid alloys. Probably the most thoroughly studied material has been the monotectoid Zn-A1 alloy.1,2,6,12,13,15 No attention to the eutectic Zn-A1 alloy has previously been reported, and the results discussed in this paper represent part of a general study of the superplastic properties of this alloy. MATERIALS The alloys used in this investigation were prepared by melting appropriate quantities of 99.99+ pct A1 and 99.999 pct Zn in air, mixing, and pouring into a water- cooled stainless-steel mold. Wet-chemical analysis was conducted with each heat of alloy prepared, using the procedure of Fish and smith.16 The composition of the eutectic alloy was 95.1 wt pct Zn. Ingots about 2 in. thick were rolled to 0.4-in. plate at about 300°C with a reduction of 5 to 10 pct per pass. Specimens were machined from the plate with the tensile axis parallel to the rolling direction. The specimens were round, with 0.150-in.-diam, 1.25-in.-long gage length, and 0.25-in.-diam threaded grip sections. EXPERIMENTAL PROCEDURE Specimens were mounted inside a uniform-temperature quartz tube which was surrounded by a double elliptical radiant furnace with a 12-in.-long uniform-temperature hot zone and a low thermal capacity. The tube extended through the top and bottom of the furnace and permitted rapid quenching of the loaded specimens when quickly filled with cold water at the conclusion of the test. The quench precluded any effects on specimen microstructure from a normal, slow cool. Constant stress was applied to test specimens by suspending a load on a constant stress cam of the type described by Hopkin.17 The design of this cam permitted application of a constant stress for elongations up to 200 pct. For greater elongation, approximately constant stress conditions were maintained by systematically reducing the load manually. RESULTS As part of an investigation of the superplastic properties of the eutectic Zn-A1 alloy, evidence was obtained for the development of elliptically shaped cross sections as originally round specimens were extended. For example, after an elongation of about 100 pct, a round specimen with an initial diameter of 0.150 in. became elliptical with major and minor axis of 0.128 and 0.88 in., respectively. Photographs are presented to illustrate the ellipticity developed during superplastic deformation, Fig. 1. The specimen shown was deformed at a stress of 500 psi, at a temperature of 285°C, and a strain rate of 2.28 x 10-2 min-1. The strain-rate sensitivity exponent* was measured at *The strain-rate sensitivity exponent, m, is defined as d In o/d In c where o is the steady-state flow stress and E is the strain rate. this temperature and in the strain rate range 10"3 to 10-1 min-1 was found to be about 0.5. This value is typical of those observed with superplastic materials. The material studied exhibited negligible strain hardening during superplastic deformation, the creep rate remaining constant under constant stress and temper-

Jan 1, 1969