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By A. R. Elsea, E. E. Fletcher

Cast X-40 alloy with the lowest nitrogen content studied had a 100-hr rupture stress at 1500°F about equal to the reported value for the commercial alloy. Increases in nitrogen content progressively decreased the rupture strength, and with about 0.1 to 0.2 pct N a minimum strength was reached, but there was no accompanying change in microstructure. Further increases in nitrogen resulted in the fomzation of progressively increasing amounts of a lamellar, pearlitic-type structure at the grain boundaries, with accompanying increases in rupture strength, and above about 0.25 to 0.33 pct N, the rupture strength exceeded the normally reported values. Two series of melts representing different melting stocks exhibited minimum rupture strengths at different nitrogen contents. This suggests that some unidentwed trace element not removed by vacuum melting has a strong influence on the response of this alloy to variations in nitrogen content. In a series of melts with manganese contents ranging from 0.6 to 3.2 pct, the material with the lowest manganese content had the highest 100-hr rupture strength at 1500°F. The manganese variations had no appreciable effect on the microstructure. CAST cobalt-base alloys such as X-40* exhibit high strengths at elevated temperatures (1500°F and above), but they also show considerable scatter in high-temperature properties. Since the design of parts for critical applications must be based on the minimum expected properties, this broad scatter appreciably lowers the design strength of the alloy. If the relatively poor properties exhibited by a few test parts from any given group could be improved, the spread in properties would be narrowed, and the design stress could more closely approach the average expected properties. The purpose of this research investigation was to learn what were the causes of these erratic properties and, if possible, to find methods for eliminating them. Earlier unpublished work showed that vacuum melting markedly influenced the high-temperature strength of cast X-40 alloy. There were indications that this behavior may have been the result of changes in the nitrogen or manganese content of the castings. Consequently, in the current investigation, the influence of variations in nitrogen and manganese content on the structure and high-temperature properties of cast X-40 alloy was studied. In this program, X-40 melting stock was vacuum melted to produce a base material that was very low in nitrogen content and in volatile trace elements. Additions were then made to this base material to produce alloys of the desired composition. The metal was cast into investment molds producing coupons which were machined into stress-rupture bars. These bars were subjected to stress-rupture tests and me-tallographic study to determine the influence of changes in analyses (nitrogen and manganese content) on the structure and properties. Material—The melting stock used for these experi-ments was in the form of shot from two master heats of commercial X-40 alloy. Only one master heat was used in a given series of melts. Thus, any differences in structure or properties that showed up in the specimens from a given series would be the result only of the intended variations in composition. The certified analyses of the master heats were as follows: C Mn Si Cr Ni Lot No. 2 0.50 0.71 0.66 25.44 10.53 Lot No. 3 0.54 0.73 0.70 25.95 10.00 W Fe Co P S Lot No. 2 7.45 1.34 Bal. 0.011 0.013 Lot No. 3 7.58 1.53 Bal. 0.005 0.016

Jan 1, 1960

By M. R. Geer, H. F. Yancey, P. S. Jacobsen

Two growing problems confront the preparation engineer—still further restrictions on stream pollution and a greater proportion of fine coal as more and more continuous miners come into use. The de-watering screens, centrifuges, and settling ponds that sufficed a few years ago must often be supplemented by more effective equipment, and in some instances the finest solids are now being recovered by vacuum filtration, once considered too costly in many coal washeries. Unfortunately not all slurries can be readily filtered. Some are virtually unfilter-able, and others do not permit the high cake rates needed to hold costs within reason. Often, however, these difficult slurries can be rendered filterable by flocculation. Starch and lime have long increased settling rate in thickeners and can also aid filtration. More recently there have been other flocculants, primarily synthetic polymers or gums. Reports of their great effectiveness prompted the U. S. Bureau of Mines to test their use in filtration as part of its program on recovering and cleaning fine coal. The object of the present work was to compare some of the newer flocculants with starch and lime and to test the reaction of different types of slurries to flocculation. Three natural slurries, three synthetic coal-clay mixtures, and five flocculants were tested, all with a laboratory filter leaf. Slurries and Flocculants Tested: First of the slurries was the thickener feed from the washed coal section of the Michel colliery of Crow's Nest Pass Co. Ltd., Michel, B.C. As shown by the screen and ash analyses in Table I, practically all this slurry was finer than 28 mesh, and about half the solids were finer than 200. Substantially all material coarser than 200 mesh was clean coal, but the ash content of 20.7 pct in the finest size indicates a moderate amount of impurity. This coal is medium-volatile bituminous in rank. Slurry was also obtained from the Black Diamond washery of Palmer Coking Coal Co., King County, Wash. This underflow of a 1/2-mm vibrating slurry screen is a waste product discharged to a settling pond. As shown by the data in Table I it contained about 20 pct material finer than 200 mesh, which analyzed 77.5 pct ash, indicating a high proportion of clay. The coarser sizes were also high in ash content because of the presence of bone and shale. Black Diamond coal is on the dividing line between bituminous and subbituminous rank. The third slurry, from the washery of Roslyn-Cascade Coal Co. in Kittitas County, Wash., was the underflow of a battery of 8-in. cyclones that is wasted with the coarser refuse from the plant. In both size and ash content this slurry was similar to the Black Diamond, but since it was a cyclone-underflow product, the fraction finer than 200 mesh undoubtedly contained a much smaller proportion of finely divided clay than was present in the Black Diamond slurry. The Roslyn-Cascade coal is high-volatile A bituminous in rank. Initially the slurry samples were stored in the laboratory at a concentration of 40 pct solids. A progressive change in filtration and flocculation characteristics during storage was noted, however, presumably because of progressive disintegration of the clay. After careful testing demonstrated that the slurry solids could be dried and then repulped without changing the original filtration characteristics, this procedure was adopted. The flocculants used were Separan 2610, Kylo 27, Jaguar MD-A, Idaho potato starch, and lime. The lime was used as a slurry, the Separan 2610 as a 0.10 pct aqueous solution, and the other flocculants as 0.50 pct aqueous solutions. The starch was causti-cized with sodium hydroxide before use. As some of the flocculants are reported to deteriorate on storage, new batches of flocculants were prepared every two days. Test Procedure: Fig. 1 diagrams the filter leaf apparatus employed. This consists of a test leaf having an effective area of 0.10 sq ft., a 60°, 8 1/2-in. diam cone to hold the slurry sample, a variable-speed electric stirrer, vacuum gage, bleed line for controlling vacuum, filtrate flask, moisture trap, and vacuum pump. Two filter cloths were selected—Saran SA 603, a monofilament, coarse-weave cloth, and polyethylene PO-801 HF, a monofilament, fine-weave cloth. The Saran was selected to provide maximum cake rate without regard to clarity of filtrate and the polyethylene to provide the best quality of filtrate without regard to cake rate. The test charge for the filtering vessel consisted of 800 g of solids (previously soaked for 24 hr) and

Jan 1, 1960

By M. C. Chang, J. Dasher

The Crucible mine in Pennsylvania, operating on Pittsburgh seam coal, is rated at 5000 tpd. The washing plant, built in 1943, is rated at about 400 tph, using hydroseparator boxes to wash the coarse coal (4 x 5/16 in.) and hydrotator units for the fine coal (5/16 x 0). It is generally acknowledged that gravity concentration equipment cannot be used efficiently to bene-ficiate coal finer than about 65 mesh. Before the present flotation circuit was installed, Crucible recovered its fine coal slurry, predominantly —24 mesh material, by passing it through a battery of five 14-in. and one hundred and ten 3-in. Hey1 & Patterson cyclones in parallel with a 75-ft Dorr thickener. About two thirds went to the cyclones and one third to the thickener. Underflows from cyclones and thickener were filtered, respectively, in one 12-disk Eimco and two 4-disk Oliver filters fitted with stainless steel cloth. The resulting cakes were added to the coarse metallurgical coal. The filtrates, overflow from the 3-in. cyclones, and thickener overflow were recycled to the coarse coal plant. The three major problems encountered in this system became acute when the mine switched from track-mounted machinery to the more economical off-track equipment. The quality and uniformity of product declined, too much slime accumulated in the circuit, and waste pond disposal became highly impracticable. Lowering of Quality and Uniformity: Since the filter cake was not beneficiated in any way, addition of this material, which contained about 18 pct ash. would certainly lower the quality of metallurgical coal. Difficulties of handling the high-ash, high-moisture cake were compounded by the lack of adequate blending facilities at the mine, making it impossible to maintain uniform feed for the coke ovens. For a two-month test period, to verify the source of trouble, all filter cake was excluded from the metallurgical coal. The excluded filter cake was stocked in the yard. Slime Buildup: The moisture retained in the coarse coal products and the filter cake provided daily the only means of slime bleed from the circuit. As this bleed was not enough to offset the incoming fines in the raw coal feed, there was excessive buildup of slimes. To operate at all, it was necessary to purge the system each weekend by pumping all the solids from the thickener to a waste pond. The slimes built up during the week progressively increased the apparent viscosity and density of the circulating plant water, so that hydroseparators and hydrotator units had to be constantly adjusted. Uniformity, yield, and quality of the metallurgical coal suffered in consequence, and the filter cake ash and moisture contents increased from Monday to Friday. Limited Waste Disposal: Location of the plant does not permit unlimited waste pond area. Maintenance of a waste pond for the purpose of emptying the thickener during weekends became a costly burden that could not be tolerated. HOW THE PROBLEMS WERE SOLVED The flowsheet (Fig. 1) chosen to overcome these difficulties is considered the one most economical to install and operate. In a preliminary change made before the flotation circuit was installed, the cyclones and thickener were first operated in series, the overflow from the 3-in. cyclones, after flocculation, being discharged into the thickener and the thick-

Jan 1, 1960

Strain-Hardening Exponent of Cross-Rolled Beryllium Sheet by S. R. Maloff, Vol. 215, No. 5, page 872, was omitted from Table of Contents for the October issue. Stabilization Phenomena in Beta Phase Au-Cd Alloys by Howard Birnbaum, Vol. 215, No. 5, page 786. The figure denoted Fig. 1 should be Fig. 3, Fig. 3 should be Fig. 4 and Fig. 4 should be Fig. 1. The captions are in the proper sequence. Activity of Carbon in Liquid Iron Alloys by Tasuku Fuwa and John Chipman, Vol. 215, No. 4, page 708. First equation, right hand column, page 710 should read

Jan 1, 1960

By L. K. Jetter, J. C. Ogle, C. L. McHargue

The preferred orientation developed in extruded aluminum rods has been studied as a function of extrusion temperature, extrusion speed, and position in the rod. Duplex <111> - <001> textures were developed for slow extrusion speeds at temperatures of 75° to 850° F and for fast extrusion speeds at temperatures of 75° to 450°F. The <001> texture component was shown to be primarily due to re crystallization occurring during fabrication. At fast speeds and billet temperatures of 650° to 850°F, complete recrystallization occurred and <115>or<118> textures were found. The nature of the structure has proved to be an important variable in the production and use of extruded products. Data on the flow of aluminum and aluminum alloys summarized by Smith,&apos; Hardy,&apos; and Locke3 show that the extruded product may possess a deformed, a partially recrystallized, or a completely recrystallized structure, and there may be important variations in the structure from surface to center and from front end to back end of an extrusion. This inhomogeneity in grain structure and preferred orientation affects both the mechanical properties of the extruded section and its response to subsequent heat treatment. Among the fabrication variables causing these differences are temperature, extrusion ratio, and extrusion speed. Preferred orientation which develops during the extrusion of rods is of the fiber-type and, in general, has been assumed to be similar to that developed in rods or wires fabricated by drawing through dies, rolling, or swaging.4 Because of the nature of the flow of metal being extruded, this assumption may be valid for material near the center of the rod but probably is not valid for the outer layers. In most face-centered-cubic metals a duplex fiber texture has commonly been reported in which the grains have either <Ill> or <001> directions parallel to the longitudinal axis. Sachs and fichiebold5 reported cold-drawn aluminum (99.6 pct pure) to have a single <Ill> fiber texture, and this observation was confirmed by Schmid and Wassermann.6 Hibbard, on the other hand, observed a minor <001> and a major <111> texture in 99.994 pct A1 cold drawn to 98 pct reduction in diam.7 He concluded that the <001> component resulted from a small amount of room-temperature recrystallization. Dayal8 concluded that the <001> component was an intermediate component which disappeared at high reductions in 99.5 pct pure Al. Kostron and schippers9 found duplex <111> — <001> textures in extruded 99.5 pct Al, as did Gow and cahnl0 and GOW11 for extruded rods of commercial and superpure aluminum. Similar duplex fiber textures have been reported for aluminum alloys by Kostron,= Unckel,13 and Van Horn.14 The present paper is concerned with the variation in texture with fabricating conditions and with the nature of the texture components in extruded aluminum rod (99.99 pct pure). EXPERIMENTAL PROCEDURE Ingots were chill-cast in cast-iron molds and machined to 3-in. diam by 6-in. long extrusion billets. These billets were upset to 3.125 in. diam and extruded through a flat-face 0.690-in. diam die. Quenching of the rods was accomplished by a water spray at the die face. The combinations of fabricat-

Jan 1, 1960

By S. Singh, R. C. Deshpande

RECENTLY metallographic studies of copper slugs recovered after firing shaped charges in deep containers of water were reported.&apos; The present note describes the metallographic examination of a steel

Jan 1, 1960

By L. G. Schulz, P. Spiegler

The electrical resistivity and the temperature coefficient of resistivity were measured with a potentiometric method using pure mercury as a reference material. Measurements were made nea,v roorn temperature. A detailed study was made of Hg,TI, near its melting temperature. THE work to be described was originally undertaken to provide the necessary data for interpreting the results of some optical experiments,&apos; but because of the growing importance of liquid metals,273 it appeared that the results of the resistivity measurements should be published separately. For convenience the alloys selected were those which are liquid at room temperature. Special consideration was given to the Hg-T1 alloy closely corresponding to Hg,Tl, because recent X-ray diffraction results of Smallman and Frost seemed to show that the solid structure may persist to some extent into the 1iquid. EXPERIMENTAL PROCEDURE A potentiometric method was employed in which the resistivity of mercury was used as a reference. The essential features of the samples are shown in Fig. 1. A capillary tube CT with a bore of approximately 1.5 mm was fitted into two end cups, T, which were made of Teflon. A pair of current electrodes CE were immersed into the excess liquid metal which partly filled the end cups. The potential electrodes PE were inserted into CT through short pieces N of a no. 18 hypodermic needle held in place with Saureisen cement SC. As shown, the lower ends of the PE7s were reduced in diameter to 0.25 mm to minimize the distortion of the liquid metal cross section. Several methods were used to insert an alloy into the sample, but the usual one with mercury alloys was to fill the sample container with a weighed quantity of pure mercury* and then add weighed the sample tube in a vacuum. Because of rapid corrosion, samples containing gallium were of necessity prepared in a vacuum. To obtain the specific resistivity of an alloy the resistance of the sample containing the alloy was measured and compared with the resistance when the container was filled with mercury. Resistances were measured in the temperature range of 20" to 60°C to obtain the temperature coefficient of resistance. The electrical measurements were made by connecting the sample in series with the standard one-ohm resistance, and the potential drop measured alternately over the sample and the standard resistance. To correct for stray thermoelectric effects provision was made for reversing the direction of the current, and the true potential drop was taken to be the average of that obtained for the two directions of current flow. Various materials were used for the electrodes, the most uniform results being obtained with nickel. EXPERIMENTAL RESULTS The numerical results are presented graphically in Figs. 2 and 3 and in tabular form in Tables I and 11. Following are remarks on results of individual alloys. 1) Hg-In—This was the first alloy studied, and

Jan 1, 1960

By R. P. Smith

Iron-carbon alloys containing a single-phase austenite region and a two-phase azcstenite + cementite region at the desired temperature were prepared by partial carburization of iron or partial decarburization of carburized iron. Each sample was held at a fixed temperature until equilibrium was achieved. Analysis of the austenite for carbon then gave the solubility of cementite in austenite. Solubility measzcrements were made for the temperature range 734° to 1012°C. These values together with other data give 7560 cal for the mean heat of solution of cementite in austenite, and 0.765 pct C for the eutectoid composition of austenite. They also indicate that graphite is the stable phase at all temperatures between the eutectoid and eutectic temperature. Measurements of the solubility of cementite in austenite at 927oand 1011 "C, using a method based on the equilibration of iron with boro-cementites, are reported. The solubility of cementite in austenite (?-iron) has been computed by Darken and Gurry1 from the observed solubility of graphite in austenite, and the thermodynamic properties of pure iron and of iron-carbon alloys. They have shown that the solubility of cementite is greater than that of graphite in the temperature range between the eutectoid and eutectic, and thus that cementite is metastable with respect to graphite and austenite saturated therewith. Since their computation is not in accord with the earlier experimental work of Mehl and wells,&apos; the present direct determination of the solubility of cementite in austenite was undertaken. EXPERIMENTAL PROCEDURE Each iron rod about 1/2 in. O.D. by 4 in. was first carburized at a temperature and with a H2-CH4 gas mixture such that the carbon content would be greater than that corresponding to the solubility of cementite in austenite at the desired (lower) temperature; sufficient carburizing time was allowed that the carbon content became substantially uniform, as illustrated by Curve A, Fig. 1. The sample was then partially decarburized with a hydrogen-water vapor mixture, giving a carbon distribution as schematically illustrated by Curve B. The sample was then held in a helium atmosphere at the temperature at which the solubility was to be determined until the decarburized portion of the sample came to equilibrium with that containing cementite. Curve C of Fig. 1 represents schematically the final carbon distribution; the horizontal portion corresponds to the carbon content of austenite saturated with cementite. To bring the sample to room temperature without change in the carbon distribution and in machinable condition, it was first quenched in a salt pot at 480°C, then in water at room temperature. Successive layers were machined from the center 2 in. of the sample and analyzed for carbon by the usual

Jan 1, 1960

By E. J. Rapperport, C. S. Hartley

I TTRIUM is a close-packed-hexagonal metal with a c/a ratio of 1.5712.1 This low c/a value prompted a cursory examination of the deformation modes to obtain more data on the deformation characteristics of hcp metals with subideal c/a ratios. The chemical analysis of the arc-melted stock from which the specimen was cut is given below in Table I.

Jan 1, 1960

By Robert Uhley, Tsvi Meidav, L. Scharon

Before National Lead built an industrial plant on its Fredricktown property, some 100 miles south of St. Louis, a 750x500-ft area on the proposed site was investigated by electrical resistivity, seismic refraction, and churn drilling. Data were accumulated to prepare an isopach map of the overburden and to determine soundness of the dolomite bedrock and the depth to bedrock at fixed points. The site was on a gently sloping hillside. Elevations above sea level ranged from 760 ft in the northwest corner to 820 ft along the eastern edge, giving a total relief of 60 ft. There were no major drainage features, but in the northern part of the plant site there was an indicated depression area which later was interpreted as reflecting subsurface conditions in the bedrock. No rock was exposed in the entire plant site area; the surface was characterized by soil and overburden. GEOLOGY Prevailing geology in the area of investigation was relatively simple—Bonneterre dolomite overlain by residuum. The red overburden was that derived from the weathered Bonneterre. Some chert was present, interpreted in the general area as a weathering of both the Bonneterre dolomite and younger sedimentary rocks such as the Potosi dolomite. During the period of actual measurements the residuum varied from moist near surface on the western edge of the proposed site to dry near surface on the eastern edge, and for this reason overburden resistivities ranged from low on the west to high on the east. Seismic velocities were low, since the material was not well packed. The bedrock encountered was dolomite, specifically the Bonneterre of Upper Cambrian age which, according to McQueen,&apos; consists of an upper dark gray member and a lower light gray member. These have been further divided into four zones, in ascending sequence a dark gray, sandy argillaceous dolomite; a dark brown or black, fine-grained dolomite: a light gray, finely crystalline, compact dolomite; and, at the top, a dark brown, finely crystalline, compact dolomite. In the area of investigation the upper two zones were encountered in the drilling tests as constituting the bedrock. The dolomite varies widely in porosity, which is low in the dense, fine-grained layers. In this area, therefore, both electrical resistivities and seismic velocities were high. Fracture zones in the Bonneterre are nearly Geology, and may extend to some depth, causing considerable deep weathering. It was realized that over deep fracturing the apparent resistivities

Jan 1, 1960

By B. G. Ricketts, A. Kelly, P. A. Beck

The isothermal kinetics (at 200" to 400°C) of subgrain growth and of softening were studied in a 99.997 pct pure Al crystal rolled to 80 pct RA, under conditions where recrystallization did not take place. It was found that the kinetics of subgrain growth and of softening were similar, and that the correlation between subgrain growth and softening was in first approximation independent of the annealing temperature. It has been shown by Heidenreich&apos; by means of electron transmission microscopy and by Hirsch and Kellar2 by means of an X-ray microbeam technique that the crystals of heavily cold-worked polycrystalline aluminum consist of subgrains of approximately 2µ diam, which are slightly disoriented with respect to each other. This substructure is found on cold working at room temperature, without annealing. A preliminary study has been previously published3 of the softening upon annealing at 350°C of a heavily cold-rolled aluminum single crystal. Softening and X-ray line sharpening for such a rolled aluminum crystal were later studied in more detail as a function of annealing time and temperature.4 Perryman5, 6 has studied the recovery of polycrystalline aluminum after cold rolling. By means of phase contrast microscopy he found that the subgrain size increases with the annealing temperature but does not alter very much with annealing time at a given temperature. In the present work further study was made of softening as a function of annealing time and temperature and subgrain sizes were determined by two different techniques in an attempt to find any correlation that may exist between softening and subgrain growth. Subgrain size measurements were made both by the X-ray microbeam technique and by transmission electron microscopy. EXPERIMENTAL PROCEDURE For the X-ray studies specimens were cut from

Jan 1, 1960

By Fred Chappell

Pyrophyllite, a hydrous aluminum silicate, physically similar to talc, receives its name from the Greek word Pyr, for fire and phyllite, a rock or stone. Firestone refers to its first recorded use as firestones or hearthstones. Composition and Properties Pyrophyllite is an aluminum silicate A12O34SiO2H2O (alumina 28.3 pct, silica 66.7 [ ] pct, water 5.0 pct) (Table 1). Vanderbilt1 gives pH value of pyrophyllite as 5.6 to 8.4. Pyrophyllite is usually white or cream, though it may be found in shades of pale green, pale yellow, buff or light gray, and in darker shades and other colors principally due to oxidation of contained iron minerals. It is opaque to translucent in thin sections. Its hardness is 1 to 2 in the Mohs scale. Its specific gravity is 2.8 to 2.9. Its luster is pearly to dull; it is recognized chiefly by its micaceous structure and cleavage, and its soft greasy feel. Two other varieties occur, one in which there are radiated needles in the crystalline form, and there is also a massive homogeneous structure found. Fine grinding reduces pyrophyllite to fiat plates or scales but aggregates of minute foliated plates may be formed.1 Distribution of Deposits Pyrophyllite is found in metamorphic rocks throughout the world but it is only in comparatively recent years that it has assumed much commercial importance. The principal

Jan 1, 1960

Established as a Society February 26, 1957 OFFICERS AND COMMITTEES Wayne E Glenn, President Earl M Kipp, President-elect John S Bell, Past President R A Morse, Vice-President W D Owsley, Vice-President Everett G Trostel, Treasurer Joe B Alford, Executive Secretary 6300 North Central Expressway Dallas 6, Texas

Jan 1, 1960

By W. A. Backofen, M. L. Ebner

SINCE the early work of Gough with Hanson and Wright,l-3 the study of fatigue has been characterized by experiments on single crystals only in recent times.9-10 Now, increasing attention is given to this aspect of fatigue research for the insight that it may provide into details of mechanism. The investigations have concentrated to a large extent on the development of deformation markings on fatigued crystals, and have shown the cracks to originate in slip bands possibly preceded or accompanied by slip-band extrusions. Experiments of special interest to the present work were conducted by paterson5 on copper crystals and involved both metallographic examination and measurement of change in flow stress. Crystals were cycled in alternating tens ion-compress ion with a constant plastic shear-strain amplitude of approximately 0.8 pct, and were particularly revealing for their demonstration of hardening with accumulated strain similar to that in unidirectional straining, through an easy-glide stage I followed by a stage II of rapid hardening; deformation was not continued beyond 40 cycles, however, so that the eventual course of the hardening curve could not be decided. For the conditions used by Paterson, surface slip markings were similar to those observed in unidirectional straining, but there were no X-ray asterisms and no deformation bands on the surface. In current thinking about the nature of fracture in fatigue, two views relative to mechanism are generally acknowledged, with the reservation that both could apply simultaneously in some measure. As one possibility, fracturing across a slip plane is regarded as a result of loss of cohesion from the creation of many point defects by dislocation movement under the cyclic loading.&apos;&apos; On the other hand, fracture has also been taken to follow as a consequence only of the geometry of slip at a free surface, consisting of offsets and crevices which eventually become fatigue cracks.12, l3 The work of McCammon and Rosenbergl4 showing fatigue in polycrystals at 4.2oK makes clear that any long-range diffusion of point defects is unnecessary, yet studies such as those of Forsyth and stubington15 show that accelerated diffusion may be a characteristic of deformation under fatigue loading. Interest in obtaining data of possible use for resolving such questions led to the experiments described below. Copper crystals were conveniently loaded in alternating four-point bending at constant deflection, a test condition shown to approximate a constant plastic strain amplitude for a wide range of axial orientations. The method of testing was not readily adapted to extensive study of temperature effects, but an investigation of the geometry of crack formation could simply be made by orienting,the slip direction at different angles to the surface. EXPERIMENTAL PROCEDURES Single crystals were grown by a modified Bridgman method in a stationary gradient furnace under an atmosphere of purified dry nitrogen. Purity of as-grown crystals was 99.999 pct as determined by spectrographic analysis plus vacuum fusion and gravimetric analyses for oxygen and sulfur, respectively. Crystals were of reasonable perfection as evidenced by a critical resolved shear stress at 10 deg from (110) of 60 g per sq mm and half-width of a (400) X-ray diffraction line from one crystal of

Jan 1, 1960

By Joseph L. Gillson

In this volume, which is divided into chapters on a commodity basis, many subjects inevitably have a common interest with others, or are interrelated in one way or another. No group of commodities is so outstanding in this regard as is that group of which the basic raw material is a carbonate rock. There are chapters in this book on dimension stone, on crushed stone, on chalk and whiting, on cement, on lime, on magnesite, on sodium carbonate; all of which are entirely, or partly, products of the "carbonate rocks." Rhodochrosite, witherite and strontianite are other carbonates described respectively in chapters on manganese minerals, barium minerals and strontium minerals; and travertine and cave onyx are carbonate materials used as ornamental stones. High grade marble is used for monuments and statues and as a decorative building stone. The aggregate tonnage of the basic raw material, the carbonate rock, is so enormous that it exceeds the tonnage of any metallic ore mined and quarried in the United States, and in turn is exceeded only by coal, sand and gravel, and by water in the gross tonnage produced by the mineral industry in this country. The specialties, including magnesite, sodium carbonate, and rhodochrosite, witherite and strontianite are produced from uncommon rock types of limited occurrence. They are described adequately in the chapters devoted to these subjects. This chapter is concerned with the limestones and dolomites. No other solid rocks are as important as these in the industrial life of the world, nor are any so widely known. Massive units of some carbonate formations form many of the spectacular features of some of the most rugged mountains in the world, such as the Dolomite Alps, the Canadian Rockies, some rugged peaks of the eastern flanks of the American Rockies in Colorado, Wyoming and New Mexico and in many ranges in Utah, Nevada and Arizona. These continue down the Sierra Oriental in Mexico and on around the world to the flanks of the Himalayas, in the South China Highlands, and separating Asia and Europe in the flanks of the Ural Mountains where they form many reexhumed hills called Shikhany.50a Less rugged and more nearly flat-lying carbonate rocks underlie most of the area of our great Middle Western plain, the southern part of England and the northern part of Africa. These are the common rock formations known from boyhood to a large part of the world&apos;s population. The use of lime, produced by the burning of limestone, goes back to antiquity, and mortar was used widely in Biblical times. The cement made by mixing volcanic ash with lime was a basic material of construction when Pompeii was built. Our Eastern states are dotted with abandoned limestone quarries, and the ruins of old lime kilns which were operated in Colonial days. Many limestones and dolomites are found in flat-lying strata of a thickness convenient for quarrying as a building stone, so that houses and other structures have been built with them for centuries. In order to replace the muddy and rutted dirt roads with surfaces that could stand the hard usage of his wagons and carts, man learned to crush stone and put a layer of it on his old trails. Such roads built by the Romans have been in use over much of

Jan 1, 1960

By M. F. Smith

BELOW the nose of the bainitic C curves in isothermal transformation diagrams, the rate of the austenite-to-bainite transformation usually decreases with decreasing temperature. However, in some steels and iron-carbon alloys, there is a noticeable acceleration in the initial reaction rate at temperatures just above Ms. Such speeding-up of the bainitic transformation would be understandable at temperatures just below Ms because of the catalytic effect of the martensite formed,&apos; but the reversal in isothermal kinetics just above Ms seems quite anomalous. This behavior was observed by Howard and Cohen&apos; in a 1.35 pct C steel and, on the basis of metallo-graphic examination, it was attributed to the formation of a thin plate-like product not belonging in the bainitic sequence. More recently, schaaber2 found two-stage reactions occurring in the vicinity of Ms in a number of steels, and suggested that the first stage might be the isothermal formation of marten-site, preceding the isothermal formation of bainite in the second stage. A decrease in the bainitic incu-

Jan 1, 1960

By R. G. Gifkins

Mean boundary migration depended linearly upon creep extension under various conditions. Prolonged annealing or air-casting increased the proportion of immobile boundaries at a given stage of tests. Grain growth during annealing followed a power law. The linking of migration and sliding in creep and models for migration are examined; activation energies are calculated from these models. Segregation of oxygen to boundaries appears to be a controlling factor. THE idea that boundary migration and boundary sliding during creep are linked has often been suggested,&apos;-5 especially when evidence has been obtained for an alternation between the two processes. In simple bicrystals sliding can occur without any migration6 but in more complex bicrystals7 it is observed. McLean&apos; and Couling and Roberts 5 made measurements of both sliding and migration; McLean concluded that there was no linking of the two processes whereas Couling and Roberts supported the idea. McLean&apos; also developed a model for migration during creep and annealing. The present work was initiated as part of a study of the recrystallization of lead during creep9 but has been extended to examine some aspects of the mechanism of migration. MATERIALS AND METHODS Specially refined high-purity lead* was used; the total of impurities, excluding oxygen, was 0.0008 wt pct. Oxygen was removed as far as possible by melting in vacuo, treating at 550" to 600°C with hydrogen and then casting at 450°C under a vacuum of 10-2 mm Hg; the oxygen was then believed to be 0.00005 wt pct. Specimens were made from extruded strip and then annealed at the required temperature in an air oven, controlled to 5 lac. They were then polished in a mixture of acetic acid and hydrogen peroxide. At this stage some specimens were etched to give grain contrast and their grain sizes determined by the intercept method. Migration of boundaries during creep was measured on the surface of polished (not etched) specimens, directly loaded at room temperature (22°C) or 50°C (52"C) to initial stresses of 300 to 700 1b per sq in. Twenty six vacuum-cast hydrogen-reduced specimens were used and, in addition, two specimens were from material air cast after hydrogen reduction ("partial" air cast) and two from air-cast material not treated with hydrogen ("full" air cast). Duplicates were made in the majority of tests. At intervals through the creep tests, specimens were unloaded and the migration measured, normal to the direction of migration at the point of measurement, for each boundary along standard traverses. Usually between 110 to 180 boundaries were measured at each of some twelve stages of the tests. Migration was measured on the projected image (X100) using prism illumination. Fig. 1 illustrates the method of measurement and shows the kind of variation of migration found from boundary to boundary and along particular boundaries. Fig. 2 gives an example of more extensive migration. The mean value of distance migrated was generally reproducible to *10 pct but occasional points gave a scatter of *20 pct. The correctibn applied by McLean8 to allow for the contribution sliding makes to the apparent distance of migration could not be used, for the sliding at most boundaries was too small to measure with the equipment available. There were two reasons for supposing the correction unnecessary in the present work;

Jan 1, 1960

By R. H. Hiltz, R. W. Douglass

Large-grain specimens of iodide titanium prepared metal-lographically were stain etched using the technique of New York University as modified by Watertown Arsenal Laboratories. Orientations of grains showing an abnormal response to stain etching were determined by back-reflection X-ray techniques. X-ray results showed that a-titanium grains, oriented such that their basal planes were parallel to the polished surface, have a slower reactivity to stain etching than any other orientation. Grains oriented such that their basal planes made small angles with the polished surface exhibited reaction rates between that of the true basal orientation and the normal rate. As the angle with the surface increases the reactivity increases up to a maximum angle of 14 deg. Basal planes making an angle with the surface of greater than 14 deg show normal reactivity to stain etching. These data, plus work on polycrystalline specimens, indicate that the oxidation rate of titanium might be reduced by correct alignment of crystal planes. ThE earliest observed phenomenon in the micrography of titanium was the occurrence of a grains which exhibited no birefringency. Even though a titanium possesses a hexagonal-close-packed structure and should be optically anisotropic, it can appear optically isotropic, when the crystal is so oriented that its intersection with the polished surface is perpendicular to the axis of symmetry. During the develoment of color staining techniques for titanium: it was noted that the a phase did not stain uniformly. Staining of specimens of commercially pure titanium resulted in a micro-structure of blue-colored grains, among which were randomly oriented a few grains exhibiting colors between the initial yellow and the final blue color. Under polarized light, these off-colored grains appeared to be optically isotropic. More intense study with polarized light, however, showed only the yellow grains to be isotropic. The intermediate colored grains exhibited weak birefringency, which at first glance is not detectable due to the strong birefringency of the surrounding structure. Aminoff2 and Straumanis3 have previously shown that in zinc the basal orientation is less reactive than other orientations. Leidheiser4 showed the same thing to be true for the hexagonal-close -packed configuration of cobalt. Thus, it would appear that the basal-plane orientation is responsible for the abnormality in stained titanium. Later work by Leidheiser5 on cobalt has shown that other planes besides the basal plane exhibited reaction rates slower than the normal rate. Reported planes were the (100), the (1011) and several planes making small angles with the basal plane. The last observance appears not to be due to the reactivity of the reported plane but due to the reactivity of the basal plane which is very close to being parallel to the surface. There are, then, two possible explanations for the range of colors observed in stain-etched a titanium. Since extensive research on the effect of orientation on surface reaction has failed to provide any definite trend, these two explanations are not adequate in themselves. Planes showing the retarded reactivity differ not only for different crystal structures but for metals of the same crystal structure and even for different reactions of the same metal. Tragert,6 Leidheiser,7 Tammann,6 and wagner9 have shown copper to exhibit retarded reactivity on the (111) plane. However, Leidheiser10 has shown that under other conditions the retarded reactivity of copper is associated with the (100)

Jan 1, 1960

OFFICERS AND COMMITTEES C C Long, President John Chipman, Past President J S Smart, Jr, Vice President T D Jones, Treasurer R W Shearman, Secretary AIME, 29 West 39th Street New York 18, N Y D C Johnston, Assistant Secretary

Jan 1, 1960

By Robert M. Grogan

Fluorspar is the commercial name for fluorite, which is the mineral having the composition CaF2, calcium fluoride. Its valuable properties are due to its content of fluorine, and it is the only important commercial source of that element. The name is derived from the Latin fluere, to flow, because the mineral melts easily and is a good flux. History The mineral has been known since Greek and Roman times, when it was used for drinking cups and ornamental slabs. Various peoples including the Chinese and the American Indians have carved ornaments from large crystals. Its usefulness as a flux was known to Agricola, who wrote about it in 1546.1 Mining began in England about 1775 15 and at various places in the United States during the period 1820 to 1840.28 Substantial production was achieved first in the period 1888 to 1900 in consequence of 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 was stimulated by growth in the steel, aluminum, chemical, and ceramic industries and accelerated by World Wars I and II. The organic fluorides called "Freons" entered the picture in 1931, and the use of anhydrous 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 1920&apos;s, a differential flotation scheme for separating fluorspar from galena, sphalerite, and other minerals in the 1930&apos;s, and the application of heavy-media concentrating methods to the treatment of low-grade ores in the 1940&apos;s were outstanding technological contributions that enabled increased production of fluorspar concentrates. Composition and Properties Fluorite in its purest form contains 51.1 pct calcium and 48.9 pct fluorine. Substitution of small percentages of cerium and yttrium for calcium have been noted.4 Mechanical inclusions of gases and fluids such as petroleum and water, and of other solid minerals such as pyrite, marcasite, and chalcopyrite are common. The fluorspar of commerce contains attached and admixed mineral impurities, chiefly calcite, quartz, barite, celestite, and various sulfides. It is interesting that the purest commercial form in which the mineral is sold, acid grade concentrate, contains a minimum of 97 pct CaF2, and as such is of comparable purity to many reagents used in chemical laboratories. Fluorite has a marked tendency to occur in large, well-formed crystals sometimes six to ten inches on a side. It crystallizes in the isometric system, frequently forming cubic and octahedral crystals or combinations thereof. The mineral also occurs in massive and in earthy forms, and in crusts or globular aggregates with radial fibrous texture. Crystalline fluorspar exhibits a great array of colors, from colorless and water clear to yellow, blue, purple, green, rose, red, bluish and purplish black, and brown. The colors are often arranged in alternating bands parallel to cube faces. They may be altered by exposure to X-rays, heat, ultraviolet light, and pressure, and are caused by a variety of factors including the presence of trace impurities and displaced ions in the lattice. Sometimes the changes induced by X-rays can be reversed by ultraviolet radiation. The mineral has a hardness of 4, and is the model of that hardness on the Mobs scale.

Jan 1, 1960