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By George Krauss, Seth R. Thomas

One complete cycle, allstenite to martensite to aus-tenite, of Martensitic transformation was induced in a commercial 18 Cr-8 Ni stainless steel. Transmission electron microscopy showed that the reverse transfarmation, martensite to austenite, perpetuated the dense defect substructure of the martensite produced by the direct transformation, austenite to 'martensite, and reproduced the retained austenite matrix orientation. A general precipitation of lathlike M,,C, particles was noted to be present in, and is suggested as cause for, regions of martensite that Izad formed after a complete cycle of transformation. The habit plane of the precipitate particles was found to be within 5 a plane previously established as the habit of nitride precipitates of similar morphology in bcc iron. The direct transformation of austenite (y) to martensite (a) in metastable 300 series stainless steels has received considerable attention in the past,'-8 and the martensite product given special emphasis in recent years,9"*u but little information has been published about the reverse martensitic transformation during which bcc a martensite is converted to fcc y austenite."-" The reversal mechanism and the resulting crystallographic relationship between parent and product austenite are of fundamental concern. The reversal product, fully austenitic, and hereafter referred to as reversed austenite, exhibits a defect structure far different from its virgin counterpart. Some studies have been reported in which the structure of reversed austenite in iron nickel alloys is compared to annealed austenite with respect to austenite strengtheningM and Stabilization.' The martensite in these Fe-Ni alloys, however, shows a basic difference from that produced in stainless steels. Structurally, the Fe-Ni martensite is profusely twinned," while the (low-carbon) Fe-Cr-Ni martensite contains a high density of tangled dislocations and is apparently twin-free.I0 reediis" has recently shown in an Fe-16 Cr-12 Ni stainless alloy that this typical martensitic defect structure and the reverse transformation directly influence the structure of the reversal product. He found that much of the reversed austenite had returned to the orientation of the virgin austenite and that fine twins were formed in the austenite after the reverse transformation. This investigation was undertaken in order to describe as completely as possible the structural changes produced by a cycle of transformation in a typical 18-8 stainless steel. EXPERIMENTAL PROCEDURE The 301 stainless steel under investigation (17.44 Cr, 7.75 Ni, 0.80 Mn, 0.60 Si, 0.40 Mo, 0.40 Cu, 0.08 C, 0.03 N, bal Fe)was received as 0.060-in.-thick

Jan 1, 1968

By M. E. Wadsworth, A. S. Peck

Infrared spectra disclose that oleic acid will not adsorb on the surface of pure beryl unless the mineral is first activated with HF. The adsorption of oleic acid on HF activated beryl is attributed to the hydrogen bonding of oleic acid monomers to F-surface bridging sites. These sites are formed as a result of the reaction of HF with chemisorbed water or surface hydroxyl. Characteristic infrared spectra of physically adsorbed oleic acid are correlated with flotation at different pH at temperatures of 25°C and 75°C for colloidal and -60-mesh particles. The usual mode of occurrence of the beryllium mineral beryl, Be3A12Si6O18, is in granite pegmatites as pale green, white, or yellow crystals. A dark green gem variety, emerald, may be found in the wall rock of pegmatite veins or in mica schist. The most important beryl deposits in the United States are in the Black Hills District of South Dakota, and several mountain ranges of central and west-central Utah contain potential commercial sources of this mineral. Several papers have been published concerning the flotation of beryl with different conditioning reagents. Kennedy and O'Meara1 reported on the essential use of HF in the flotation of beryl from different ores. The use of calcium hypochlorite to separate HF activated beryl from feldspar after flotation with an amine collector was made by Runke.2 A report on the activation of beryl with different cations using sodium oleate collector was presented by Viswa-nathan and co-workers.3 Flotation of beryl with sulfonate collector and different activating salts was employed by Fuerstenau and Bhappu.4 The role of the surface charge or zeta potential in the flotation of beryl with different collectors and salts was also extensively investigated.5"7 Previous infrared investigations by the authors8 disclosed that the orthosilicate beryllium mineral, phenacite, reacts with oleic acid to form a chemisorbed oleate monolayer on the mineral surface. Thus, chemisorption is the effective mode of adsorption in the phenacite-oleate acid flotation system. In contrast, neither chemisorption or physical adsorption of oleic acid occur on the surface of pure beryl as evidenced in this study. Efforts were subsequently made to determine the mechanism of activation and collector adsorption for HF pretreated beryl. EXPERIMENTAL PROCEDURES Large, white, terminated crystals of beryl were obtained from Madagascar through Ward's Co., Monterey, Calif. The crystals were broken into -60-mesh fragments in a porcelain mortar. Part of this prepared material was ground to a powder with a Fisher Grinder using an agate mortar and pestle. The powder was transferred to a graduated cylinder and mixed with 500 ml of distilled water. After 5 min, the colloidal suspension was separated from the settled particles by decantation and used as a stock for infrared test determinations. Adsorption tests were performed by first transferring 20 ml of colloidal suspension to 50 ml glass centrifuge tubes. The solids were then centrifuged out and the liquid was discarded. Then, the solids were pretreated with one molar HC1 or one molar HF. After 15 min, the solids were again centrifuged out. The mineral solids were washed free of residual acid by repeated centrifuging and water washing operations. Then, 20 ml of distilled water was added to the solids, and the resultant suspension was used for test purposes. In the preparation of mineral for flotation tests, 1.5 g of -60-mesh beryl was deslimed by removing the colloidal fraction by three successive water washes and decantations. Then, the coarse particles were pretreated with either one molar HCl or one molar HF for 15 min. The mineral was next washed free of acid with distilled water, and 20 ml of distilled water was added to the beryl prior to collector conditioning. The conditioning of mineral with collector was performed in 50 ml centrifuge tubes to which either NaOH or HC1 was added for pH modification. One drop (6.0 mg) of U.S.P. reagent grade oleic acid or 2 ml of 0.01 molar sodium oleate was added to the pulp and stirred at about 1500 rpm for 3 min at a

Jan 1, 1968

By Frank G. Snyder, Paul E. Gerdemann

The Southeast Missouri lead district, located about 70 miles south of St. Louis, embraces four important sub-districts and several minor ones. The important sub-districts, in order of discovery, are Mine La Motte, the Old Lead Belt, Indian Creek, and the Viburnum Lead Belt. Descriptions that follow are of geology and ore deposits of the Old Lead Belt. The ore deposits are stratiform in character and are localized in a narrow carbonate bar and algal reef environment on the flanks of exposed Precambrian of the St. Francois Mountains. Ore structures include a variety of primary depositional features such as pinchout zones, disconformities, ridge structures, reefs, and submarine gravity slides. Faulting, prior to and during ore deposition, "prepared" the host rock and strongly fractured areas are mineralized much more intensively and extensively than unfractured parts of the same sedimentary structures. The deposits are epigenetic in character. Mineralization is believed to have occurred at the time that post-lower Ordovician faulting took place. The mineralizing solutions are believed to be concentrated brines from adjacent basins that moved out of the basins during faulting, uplift, and erosion of the St. Francois positive area.

Jan 1, 1968

Jan 1, 1968

By Leo J. Vogel, E. D. Hummer

INTRODUCTION by E. D. HUMMER An efficient refuse-disposal system is a necessary part of the modem cleaning plant. The large-scale refuse system and disposal area, engineered for the lifetime of the plant, has become more important due to the greater tonnages of refuse produced from increased quantities of mechanically mined and prepared coal. Laws and increased government regulations have affected the design and operation of disposal systems. THE EFFECT OF MINE AND PLANT OPERATION Refuse disposal starts at the mining face. The mining system, the type of roof support, the machinery used, and the degree of discipline at the face contributes to the amount and type of refuse that must be removed through the disposal system. Economies gained through modification of the mining system or mining machinery may be partially offset by increased dilution of the mined coal with impurities from associated rock formations. In some cases the change in the mining system and equipment has reduced the dilution. In all cases the ratio of impurities that must be removed from the raw-coal feed to the plant not only affects the maintenance and operating costs of the plant, but greatly affects the design of the refuse disposal system. The design of a mine and plant should include the location and the estimated capacity of the disposal areas for the life of the property or plant. Complete evaluation of the disposal system and an estimate of its annual cost of operation over the life of the property or plant should be incorporated in the plant and mine evaluation. Plant design should be as simple as possible, consistent with the efficient production of clean coal. Material transfer points, crushing, screening and pumping operations should be kept to a minimum to reduce degradation and the subsequent increased difficulty and cost of refuse removal. The maintenance of good process control by operating management will result in a minimum of misplaced material in both refuse and clean coal. Reduction of misplaced float material in the plant refuse is an important factor in preventing combustion in the refuse storage pile. THE REFUSE DISPOSAL AREA Combustion in refuse piles occurs when air enters the pile in sufficient quantity to support oxidation. At certain rates of air in-filtration, the heat produced by the oxidation process is not dissipated and temperature rises.

Jan 1, 1968

By I. J. Hegyi, J. J. Tietjen, H. Nelson, J. I. Pankove

The fabrication of p-n junctions in GaAsl-,P, alloys by a vapor-phase gowth technique has for the first tirne resulted in room-temperature injection lasers capable of operating over a broad range of wavelengths extending into the visible region of the spectrum. The shortest wavelength achieved to date is 6750A at room tetnperature. In addition, at 78°K the threshold current density values for these lasers are generally the lo~vest reported, and the emitted radiation extends to the lozc,est wavelength ever attained (6350A). With lasers fabricated from material containing 14 pct Gap, quanticm efficiencies of 26 pct and peak power outputs of 25 zu were obtained at room temperature. ALTHOUGH room-temperature operation of GaAs injection lasers has been well-documented,&apos;-5 the operation of GaAsl-,P, (x > 0) laser diodes has been restricted to relatively low temperatures.8-&apos;0 This has been previously attributed5, 7, 10-12 partially to the difficulty of preparing single-crystalline GaAsl-& alloys having a high degree of chemical homogeneity and purity. Also, with these materials it has been difficult to prepare high-quality, abrupt p-12 junctions by diffusion techniques; and, in turn, this has made it difficult to obtain optimum electrical properties for room-temperature operationL3 in the resulting laser diodes. As a result, GaAsl-,P, laser diodes have not been efficient enough to permit operation at room temperature. For example, using diffused structures, only a few diodes were obtained which could be operated even close to room temperature (255K)." Recently, a vapor-phase growth method of preparing epitaxial deposits of GaAsl - .P, alloys has been described,14 and the high-purity and homogeneity of these materials has been previously demonstrated. Of special significance, with this technique, n- or p -type doping can be initiated or discontinued at any time and at almost any rate during the crystal growth so that the donor and the acceptor concentrations can be easily controlled to obtain desired impurity profiles. This permits high-quality, abrupt p-TZ junctions to be vapor-phase grown entirely during the crystal growth process, so that diffusion or other p-n junction fabrication processes are unnecessary. After growth, the device does not have to be heated to elevated temperatures, which avoids the possible unwanted introduction and motion of both impurities and lattice defects. Using the vapor-phase growth method cited above, over 300 room-temperature injection lasers have been prepared from GaAsl-,P, alloys having compositions in the range of 0 5 x 5 0.41. These lasers have emitted cohe~ent radiation in the spectral range of 8350 to 6350A at 78°K or from 9000 to 6750A at room temperature. The threshold current densities of the best lasers are independent of the alloy composition over the range 0 < x < 0.2 and compare favorably with values for good GaAs lasers.&apos; MATERIAL PREPARATION Multilayer, epitaxial deposits of GaAsl-,P, alloys are prepared by a vapor-growth technique described elsewhere.14 With this technique, the individual layers which comprise the multilayer structure are prepared sequentially in the deposition apparatus without interrupting the crystal growth. The epitaxial layers are deposited on GaAs substrate surfaces oriented normal to the ( 100) direction. The substrate wafers employed in this study were usually doped with tellurium to an electron concentration of approximately 2 x 10" per cu cm. To avoid strains, the first 10 to 15 p of the deposited material is uniformly graded from pure GaAs to the specific GaAsl- ,P, alloy composition of interest. The GaAsl - ,P, alloy growth is then continued to form a layer of constant composition having a thickness in the range of 25 to 75 p. Both the graded region and the layer of constant composition are doped with selenium to an electron concentration of about 2 x 10" per cu cm. The p region of the diode is then incorporated in the crystal by abruptly changing the dopant concentrations in the vapor phase to facilitate doping with zinc. This layer has a hole concentration of approximately 3 X 1019 per cu cm and typically is 50 p thick. DEVICE FABRICATION In general, the GaAs substrate and the region of graded composition are removed. Ohmic contacts are made to the n-type side by tin evaporation and to the p-type side by an electrodeless nickel deposition. This is followed by an electrodeless deposition of gold on both sides. The crystal wafer is then cleaved along (110) planes and sawed into rectangular parallelepipeds. Typical dimensions are 100 by 300 for the junction area and 100 µ for the diode height. The diodes are either soldered to a copper stud or pressure-mounted in a copper clip. RESULTS AND DISCUSSION Approximately 400 laser diodes having compositions in the range of 0.41 have been prepared by the method described above. Each laser was routinely tested at liquid-nitrogen temperature. The lasers were operated with l-psec current pulses at a repetition rate of 60 pulses per sec. The parameters of greatest practical interest are the photon energy or wavelength of the laser output and the threshold current density. Fig. 1 shows the variation of photon energy with alloy composition at 78°K. The composition was determined from the lattice constant of the material obtained by X-ray back-reflection measurements. Although there

Jan 1, 1968

By B. J. Bayles, J. A. Ford, M. J. Salkind

Unidirecltonally sulidijied AL-A13Ni was found to exliibit excellent microstructural stability to 508°C. Above this temperature the transverse micvostructure coarsened in a manner analogous to "Ostwald Ripening", but the A13Ni whiskers did not spheroidize or foreshorlen. The coarsened whiskers reinforced the matrix as effectirely as the finer whiskevs and no reduction in room-temperature tensile strength mas noled after exposure for 90 hr at 96 pel 0-1 the absollite melling temperature of the eulectic. The slability was auribucted to the presence of low-index (and presurrlably lor-energy) cvystallographic interjaces between phases. The driving force for microstructural coursening was presumed to be the reduction of interfacial energy between the phases. Finer micvoslructures were found to coarsen more rapidly than those which weve imitally coarser. FIBER-reinforced metals have been shown to exhibit good short-time tensile properties at elevated temperatures.1-4 However, many elevated-temperature applications require long-time property retention which dictates the necessity for microstructural stability. Two types of instability are common to fiber composities. The first, chemical instability, is due to chemical reaction between the matrix and the relnforcing phase. Petrasek and weeton5 have shown that chemical reaction between tungsten wire and several copper alloy matrices resulted in degradation of the reinforcing phase and reduction in strength of the composite materials. Kreider and Leverant4 have noted similar behavior for boron-reinforced aluminum above 400°C. The second type of instability arises in systems in which the phases are essentially chemically stable with respect to each other and is characterized by spheroidization and/or agglomeration of the reinforcing phase. parratt6 has reported this type of degradation to occur relatively rapidly at moderate temperatures for nickel and cobalt alloys containing whiskers of silicon nitride, aluminum oxide, and silicon carbide and has identified it as "physicochemical" instability. Although both types of instability are the result of the differences in the chemical potential between the fibrous phase and the matrix, they may be differentiated by the fact that the second type, "physicochemi-call&apos; instability, results in little or no net change in the composition or amount of each phase present. It does, however, result in a morphological change which profoundly affects the strengthening mechanism. Chemical interaction. on the other hand, results in a change in the composition and amount of one or more of the phases present, or the appearance of a new phase. In the latter case, the appearance of the mi-crostructure, that of a fibrous phase aligned in a matrix, may remain essentially unchanged, but the chemical degradation of the fiber results in markedly reduced composite strength. This investigation was initiated in an attempt to evaluate the microstructural and related mechanical property changes of a whisker-reinforced eutectic composite after elevated-temperature exposure. The composite system chosen for this study was the uni-directionally solidified A1-A13Ni eutectic which Lemkey. Hertzberg, and Ford7,8 demonstrated to behave as a whisker-reinforced composite. The microstructure of the unidirectionally solidified material consists of aligned needles of A13Ni in a matrix of aluminum. EXPERIMENTAL PROCEDURE Eutectic ingots having a nominal composition of 6.2 wt pct Ni were produced by melting 99.99+ pct A1 and 99.99 pct Ni in recrystallized alumina crucibles in an argon atmosphere. The analyses of the starting materials are listed in Table I. These master heats were cut up? melted by induction heating, and unidirectionally solidified vertically in 1/2 -in.-ID. 6-in.-long graphite crucibles, in a dynamic argon atmosphere. Therma1 gradients in the liquid were determined by measuring the temperature in the melt as a function of apparatus travel distance, as discussed by Kraft and Albright.9 The rate of solidification was assumed to be equal to the uniform rate at which the crucible assembly was withdrawn from the furnace. Ingots representative of nominal growth rates of 2, 5, and 11 cm per hr were produced and the solidification parameters are summarized in Table 11. Ingots used for met allographic analysis were pre-

Jan 1, 1968

By B. K. Asdell

Crude kaolin exhibits a wide particle size range in which kaolinite is the predominant mineral. Bene-ficiation by wet processing produces high-brightness white pigments. The wet processing techniques peculiar to kaolin beneficiation are emphasized in this article in some detail. Included are discussions of long-distance pipeline transportation, centrifuga-tion, flotation, spray drying and shipment as 70% solids slurry. Georgia, a state seldom considered to be an important mineral producer, has one surprising feature — it is the nation&apos;s largest producer of kaolin. Kaolin is a highly important raw material in the paper, rubber, ceramic whiteware, paint and chemical industries. In 1965, more than 2.7 million tons of kaolin were produced in this state, a 150,000-ton increase over the preceding year, and production continues to climb. Strictly defined, the term "kaolin" applies to a group of hydrous aluminum silicates in which kaolinite is the predominant mineral. Kaolinite is inherently white, non-abrasive, chemically inert, and of a very fine particle size, ranging from sub-micron to 40-microns equivalent spherical diameter. An electron-micrograph of kaolinite is shown in Fig. 1. The particles finer than about 2 microns are thin, elongated plates, hexagonal in outline. The larger particles, coarser than 2 microns, are predominantly vermicular in outline with a foliated structure. Table I shows a typical chemical analysis of commercial, wet-processed kaolin compared to pure kaolinite. The sedimentary Cretaceous deposits of the Coastal Plain are the source of most of the kaolin produced in the Southeast. These deposits are of relatively high purity, and it is not uncommon to find the clays running greater than 90% kaolinite. Beneficiating plants using wet processing techniques are most numerous in an area within about 50 miles east of Macon, Ga., in a band approximately 15 miles wide. Kaolin may vary widely in quality from one deposit to another, or within the same deposit. The qualities critically examined are brightness index as measured by reflectance, viscosity of water suspensions, bleachability and particle size distribution. Crude kaolin always contains sand and mica in varying amounts, along with small amounts of many other minerals. These are classed collectively as "grit" because; they are generally coarser than 325

Jan 1, 1968

By R. Lagneborg

WhEN mechanical twins initiate cracking it has been proposed1 that the friction stress for dislocation motion, in the Cottrell criterion for brittle fracture2 should be replaced by the stress required to propagate a twin, ttp. TF is the fracture stress, d the grain diameter, ß a geometric constant, u shear modulus, and y the effective surface energy. Since TTp is likely to vary with grain size, it cannot be substituted by a constant in Eq. [I]. If an expression for the energy change caused by a twin in a stressed material could be obtained, it is in principle possible to compute the critical size of the twin, i.e., the size at which the system can decrease its energy spontaneously, as a function of applied stress, thus giving the stress required to just barely propagate the twin, i.e., TTP. Consider a circular twin disc with a radius r and having a lenticular cross section, Fig. 1. Twin dislocations3 of strength b exist in the twin boundary parallel to the twin plane, one loop on each atomic plane. Assume that the total numbers of loops, n, can be replaced by one circular loop of a multiple dislocation, nb with a radius r. The energy change of the system, AW, due to such a twin in an applied stress field can then be calculated: The first term is the total twin surface energy, the second the elastic energy due to the twin dislocations, and the third the energy released by the twin in the applied stress field. yt is the twin boundary energy, r, the radius of the dislocation core, and T the applied

Jan 1, 1968

By V. Patarini, M. Salkind

BECAUSE of its high strength and stiffness coupled with low density, continuous boron filament is showing great promise as a potential reinforcement for both metals and nonmetals. Of primary consideration for structural applications is the fatigue behavior of boron fiber composites. Composite fatigue behavior is dependent upon three factors: 1) fiber fatigue behavior, 2) matrix fatigue behavior, and 3) the effect of the interface and fiber ends. The purpose of this note is to describe the behavior of boron filament in rotating beam fatigue. The filament, described by Talley&apos; and Galasso, Salkind, Kuehl, and Patarini,&apos; was made by the hydrogen reduction of boron trichloride on a hot tungsten filament. Testing was performed using a commercial rotating beam wire fatigue tester* described by Votta.~ One end of the test sample is held in a chuck in a synchronous motor. The sample is bent around in a "U" shape, and the other end inserted into a carbide bushing. The maximum strain occurs at the bottom of the "U" where the radius of curvature is a minimum. The strain is adjusted by adjusting the length of the specimen and the location of the bushing. Samples were rotated at 3600 rpm and an automatic shutoff device used to determine the number of cycles to failure. The measurements were accurate to the nearest 360 cycles. The fatigue behavior is summarized in Fig. 1 for fifty-one samples of 4.8 x 10"3 in. diam fibers and ten samples of 3.2 X 10"3 in. diam fiber. The two sample groups represent two different filament production runs and two different nominal size groups. Both groups exhibited nominal tensile strengths of 400,000 psi. No significant difference in the fatigue behavior of the two sample groups is apparent. The scatter in the data is not unexpected for a brittle filament which exhibits a tensile strength distribution with a standard deviation of 10 to 15 pct. Because the test procedure provides a known outer fiber strain in the sample, the maximum stress was calculated assuming a Young&apos;s modulus of 58 x 10&apos; psi. This value was selected as being representative of several nominal fiber sizes.2 All of the samples which failed exhibited sudden, catastrophic fracture, and no permanent deformation. One sample was stopped after 1.66 x lo8 cycles at *200,000 psi. The fiber exhibited no apparent damage or deformation. It is apparent that the fatigue resistance of boron filament is quite good. It can therefore be speculated that the fatigue behavior of boron fiber composites would be controlled by the "weaker links", namely matrix fatigue resistance and interface behavior. In fact, preliminary investigations have revealed that this is true for boron-reinforced aluminum? It should be noted that the data presented herein may not necessarily reflect the tensile fatigue behavior of boron filament. It is well-known that boron filament has a radial residual stress pattern with the outer surface in ~om~ression.~ Because of this fact, tensile failure is normally nucleated in the interior of the filament.5 Since the data presented herein is for a rotating beam test in which only the outer surface of the fiber is stressed to the maximum value, it would be incorrect to assume that the failure mechanism and fatigue behavior would be the same if the fiber were tested in tensile fatigue. The fact that many of the data are well above the nominal 400,000 psi tensile strength would tend to support this argument. The authors would like to express their appreciation to the United Aircraft Research Laboratories for supporting this investigation and for permission to publish the results. A portion of this effort was supported by the Air Force Materials Laboratory under contract AF33(615)-2125.

Jan 1, 1968

By T. F. Bower, M. C. Flemings

Results are reported of a study of surface dendrilic structure of an Al- Cu alloy solidified against a chill wall. Most primary and secondary "arms " in the surface dendritic structure are arranged orthogonally, giving the impression of strong preferred orientalion on the surface. However, no such preferred orientation exists and it is therefore evident the arms do not represent (100) directions. The primary arms are shown to be interseclions of a (100) plane wilh the chill plane, or, equally often. the projeclion of a (100) direction on the chill plane. Secondary dendrite arms are usually within a few degrees of 90 deg to the primary arm, independent of grain orientalion. Prirary, secondary, and higher-order surface dendrite arms almost always represenl intersections of (100) platzes with the chill surace, or pvojections of (100) direclions. Growlh of secondary arms is favored on the side of the primary arm where a (100) direclion points toward the chill surfAce a1 a Lou, angle. Surface dendrile arms are often observed to be bent. In these cases, the crystal lallice changes orientation; bending is concave to the chill surface. In a previous paper,&apos; a technique was discussed whereby large grains can be obtained at a chill surface. The technique used involves quickly drawing superheated liquid A1-4.5 pct Cu alloy into a thin copper mold, so that the mold is full well before solidification begins. The chill surfaces employed are polished copper blocks coated with amorphous carbon. Shrinkage during solidification between dendrite arms and grains delineates both, without the need for polishing or etching of the cast surface. The grain structure of the chill surface was discussed in a previous paper;&apos; in this paper, the dendrite arms within each grain are examined. Previous work on surface dendrites includes that of Edmunds, who studied the development of preferred orientation in zinc, cadmium, and magnesium.&apos; In zinc and cadmium, he found that the surface region has a (0001) texture (parallel to the chill surface). Walton and Chalmers reasoned that, since the fast growth (1010) directions are in the basal plane, nuclei which have this plane parallel to the mold wall would produce larger grains than nuclei with other orientations. Hence, the texture observed is as expected.3 The same authors, in measurements on aluminum ingots, found no preferred orientation at the mold wall. However, the X-ray technique they used measured the preferred orientation in terms of grain numbers, not grain areas; larger grains were weighted equally with small ones. No preferred orientation is expected on this basis at the chill surface. In a later paper,&apos; Edmunds stated that experiments show a random grain orientation at the surface in die cast aluminum; his technique, also used in his earlier paper, takes account of grain area. Little work has been published on the dendritic structure of metal chill grains. Recent work of Biloni and Chalmers on "predendritic growth" shows the change in morphology from spherical to dendritic during the initial stages of freezing, 5 but this work did not include detailed examination of the fully developed dendrites. Other pertinent work includes that of Lin-denmeyer, who investigated the growth of ice dendrites. 6 When growth was on a substrate, the dendrite axes were bent. The bend corresponded to a change in orientation of the crystal lattice and occurred in such a way as to align the basal plane to the substrate. DENDRITE STRUCTURE Fig. 1 shows the chill surface of a typical casting poured above the critical temperature necessary to produce coarse grains. A cursory examination of these grains shows that the surface dendrite arms within most of the grains are oriented roughly perpendicular to each other. One is tempted to assume that these are (100) directions and that, therefore, marked preferred orientation exists at the chill face. This, however, is not the case. Each of the grains in the casting of Fig. 1 was separately identified, Fig. 2, and its orientation determined by the Laue back-reflect ion method. Results are given in Fig. 3 and it is seen there that no preferred orientation exists. Even when grain area is accounted for, there is no significant preferred orientation. The relationship between surface grain structure and crystal orientation was then obtained by assigning X and Y axes to the casting surface, Fig. 1, and assigning the same axes to the stereographic projections of each grain. Thus, the visible surface structure could be compared readily with grain orientation. This was done for fifty-five of the grains of Fig. 1. Results of this study on three typical grains are described below, and some general observations given subsequently. Fig. 4 shows the structure and stereographic projection of a grain which lies near the (100) zone (with respect to the casting surface). The X and Y directions are marked on the projection, and the photomicrograph mounted with the same orientation. Poles of the stereographic projection represent crys-tallographic directions in the grain which point out of the casting, toward the chill. Two (100) directions are shown in Fig. 4. A line joining the center of the projection and a pole represents the projection of the pole onto the X-Y plane (chill surface). Two such lines are shown in Fig. 4 (solid lines). A line joining the intersection of a great circle with the circumference of the projection gives the trace of a crystallo-graphic plane in the chill surface; two such traces are shown (dashed lines).

Jan 1, 1968

By M. C. Fuerstenau, W. F. Cummins

The flotation response of quartz in the presence of calcium chloride and various fatty acids is presented. Flotation is not effected with lauric acid until calcium laurate is precipitated in solution, while flotation is obtained with the 9, 10, and 11-carbon members before precipitation of the calcium carboxylate. The active species responsible for flotation is suggested to be a basic aqueous complex, e.g. Ca(OH) (RCOO) (aq), and a possible mechanism of adsorption is given. Most of the previous work on activation in non-metallic flotation systems has involved the use of high molecular weight collectors, such as oleic acid or alkyl aryl Sulfonate.1-7 In these studies the levels of addition of collector and activator required for flotation were much above the concentrations necessary for precipitation of the metal-collector salt. In fact, Clemmer, Clemmons, Rampacek, Williams, and Stacy1 have stated, "Our experiments on a variety of materials have demonstrated that the metal salts which react with anionic collecting agents, as soaps and alkyl sulfates, to form relatively insoluble compounds may be employed as activating agents provided an optimum quantity is used at a proper pH." On the other hand, Gaudin and chang8 obtained flotation with additions of barium and lauric acid below the level required for barium lautate precipitation.

Jan 1, 1968

By R. C. Hall

We are pleased to confirm some of the mechanical data presented by Dr. Detert on the 18 pct Ni marag-ing steel.15 Bar 3 in. in diam and containing 0.02 wt pct C, 18.5 Ni, 8.9 Co, 5.1 MO, 0.55 Ti, 0.05 Al, and balance iron has been examined in our laboratory. Cylinders 0.5 in. high and 0.4 to 0.5 in. in diam were cold-compressed from 3 to 40 pct reduction in height. Table VI shows some typical data; deformation in-

Jan 1, 1968

By J. F. Held

In a study of the influence of cold rolling on mechani cal properties of steel, it was found that the specific rolling procedure influenced crystallographic orientation. Properties developed by several rolling modes were determined and related to crystallographic orientation. Sanzples were cold-rolled various amounts on a laboratory mill. When palm oil was used as a lubricant, the crystallographic orientation was homogeneous throughout the thickness of the samples. Other samples were rolled without lubrication. Variations in intensity of the recrystallization texture components persisted throughout more than 50 pct of the volume of these samples. When the average plastic strain ratio, which is dependent upon crystallogvaphic orientation, was plotted as a function of percent reduction, a maximum was found at 40 pct in the samples which contained the observed texture variation. No maximum was found for the samples with the homogeneous texture distribution. Other mechanical properties, such as tensile strength and yield strength, were not influenced by the variation in crystallopaphic orientation. MECHANICAL properties of steel sheets depend, in general, upon the structural properties of the steel. For example, the Petch equation describes the relationship between yield strength and grain size. Other properties, such as hardness, vary with chemical composition. The plastic strain ratio, or R value, has been found to be dependent upon crystallographic orientation . In the course of investigating the effect of cold rolling on mechanical properties, it was found that a previously reported relationship between percent cold reduction and R value was not always observed. Published data had shown that the optimum cold reduction for best R values is 70 pct for aluminum killed steel.&apos; However, by altering the rolling conditions, the optimum reduction can be shifted to much lower values, or it can be moved to very high values. This paper describes the rolling conditions that lead to shifting of the optimum cold reduction. The effect of rolling conditions on the various structure parameters and the resulting mechanical properties are evaluated. EXPERIMENTAL PROCEDURE Samples of three low-carbon aluminum killed steels were cold-rolled various amounts on a 9-in.-diam 2-high laboratory mill. Hot-mill thermal practice and steel chemistries are listed in Table I. Steel A was rolled with palm oil lubrication and heavy reductions on each pass; i.e., a total reduction of 75 pct was ac- complished with a maximum of five passes. Steel B was rolled without lubrication, and light reductions were given on each pass. After approximately 75 pct reduction, it was necessary to use a small amount of light oil to achieve any additional reduction in thickness. Following cold reduction, the samples were box-annealed at 1300°F for 10 hr. The heating rate between 800" and 1300°F was 50°F per hr, and the cooling rate following the soak period was 50°F per hr. Tensile specimens were machined from the annealed material and these were used to measure yield strength, tensile strength, and the plastic strain ratio (R value). Recrystallization textures were determined by an inverse pole figure technique.*&apos;3 Integrated intensities of the (110), (002), (112), and (222) reflections were recorded for those planes lying parallel to the sheet surface. Examinations were made on both surfaces of each sample, and also at various levels beneath each surface to approximately 0.010 in. depth by etching techniques. RESULTS R Values. The R values obtained in steels A and B are shown as a function of percent cold reduction in Fig. 1. No optimum cold reduction was observed in steel A, rolled with palm oil lubrication. It is likely, however, that an optimum reduction would have occurred had higher reductions than 88 pct been employed. The optimum reduction in steel B occurred at 40 pct. The behavior in both of these steels is quite

Jan 1, 1968

By W. Henry Weimer

A successful surface coal operation requires the combined efforts of engineering and operating personnel. In the planning for a mine, machines should be selected to do the best work in getting the coal uncovered, loaded, and transported to the preparation plant. The best system and extent of cleaning will be determined by the market. After the fundamentals of operation have been established, the operating personnel should see they are carried out. There is no simple solution to some of the every day problems facing the operating officials. Here the production engineer with the technical approach, time studies, control methods, past experience, and available records can help in detecting causes of inefficient phases of the operations. With these studies, a careful analysis can be made in setting up the expected standards to be followed. Management can then compare the job under study with the standards and make corrections to solve the problems. 5.2-1. Annual or Daily Coal Production. Once the production cycle has been established, it is paramount that coal sales keep the productivity of the mine as high as possible. A successful company does this by what they call "the control approach." The daily tonnage report is one of the things that is a potent control tool in attaining the goals to be achieved. If production is falling short of the goal, the daily tonnage report will reveal what has to be done in the remaining days of the month or year to achieve the expected schedule. When goals are reached or exceeded, then budgeted tonnages and costs will be reached or exceeded and thus assure attainment of a profit. Failing to keep to the scheduled pace shows up quickly and prominently, facilitating any necessary action to get things back to the projected plans. The sales target is usually set a little higher than the operating production. The sales tonnage is scheduled and sales are made accordingly, slightly

Jan 1, 1968

By David Phillips, George Jura

WHEN Bridgman1 determined the volume-pressure relationships of bismuth to 100 kg Cm-2, he found two small volume discontinuities at 45 and 64 kg em-2. Probably every investigator in high pressures has determined the electrical resistivity of bismuth in this pressure range. Until Zeitlin and Brayman2 reported discontinuities in the resistance of bismuth at these pressures, no one had found resistance discontinuities

Jan 1, 1968

By John R. Hutchins

1ms is a report of nickel (wire) oxidation studies designed to test the validity of Valensi&apos;s1 equation developed for the kinetics of a reaction controlled by diffusion in a continuously growing product layer on cylindrical surfaces. The equation is:

Jan 1, 1968

By Barry K. McMahon

The fundamental problem in rock mechanics is accounting for the discontinuous and anisotropic nature of the jointed rock mass. It is this problem that makes rock mechanics distinct from the mechanics of steel, glass, or concrete. Existing mathematical models explain much of the behavior of rock cores in the laboratory but, in civil engineering at least, the rocks that matter are the ones that are already broken. On the other hand, the basically descriptive methods now used in engineering geology do not lend themselves easily to mathematical analysis. A set of indices of geological properties related to the strength and deformation characteristics of jointed rock is needed. Like the index properties used in soil mechanics these will probably not have precise mathematical meaning, but once correlations are established with large scale tests they can form a basis for the transfer of test results, obtained in one area under one set of conditions, to the prediction of rock behavior in another area under another set of conditions. Indices of rock properties are even more important in rock mechanics than in soil mechanics as the cost of testing is much higher. To be useful, these indices must be easily and quickly measured and give reproducible results when measurements are made by different people. In this paper the word "joint" means all naturally occurring rock fractures with less than 3 in. of clay or other soft coating material. EXISTING INDICES OF ROCK PROPERTIES A comprehensive review of indices of rock properties for intact rock is given by Deere and Miller.&apos; They provide charts ". . . for estimating the strength or modulus properties for intact rock from the numerical indices obtained by either the Schmidt hammer, the Shore Scleroscope,

Jan 1, 1968

By Maurice Magee

The Ducktown ore deposits have been known, explored, and mined for 120 years. Eight massive sulfide ore bodies occur in highly folded and metamorphosed graywacke, graywacke conglomerate, mica schist, chloritegarnet schist, and staurolite schist of Precambrian age. The ore deposits are tabular bodies that have been extensively folded, generally conform to the enclosing rocks, but show local complex differences. The ore deposits, ranging in size from 250,000 tons to over 20 million tons, are composed principally of the minerals pyrrhotite, pyrite, chalcopyrite, sphalerite, and magnetite. Gangue minerals are quartz, calcite, actinolite, tremolite, hornblende, garnet, and masses of schistose wall- rock. Three fault systems are present that have influenced ore control and ore body configuration. Hydrothermal effects are evident in wall-rock alteration. Evidence of retrograde metamorphism is extensive in the wall and ore associated rock. Preliminary isotopic age dates have indicated four possible metamorphic events during the Paleozoic Era. Ore genesis is considered to be hydrothermal replacement of receptive beds, predominantly highly calcareous zones, quartzitic zones, and brecciated shear zones. Ore deposition is thought to have occurred during the Devonian Period, with later mobilization and recrystallization of the ore and gangue during Middle and Late Paleozoic times.

Jan 1, 1968

By Victor A. Phillips

A series of strips of a Ni-12.7 at. pct A1 alloy were Prepared containing cubical y&apos;(NisAl) precipitates with edge lengths from 60 to 500A. A particle-free solution-tveated strip was included for cornparison. They weve cold-rolled 95 pct and the effects of particle size on the isochronal (1/2 hr) annealing behavior between 300° and 950°C studied (by hardness and light and electron microscopy). It ulas inferred that the particles deformed with the lnatvix becoming lamellae which remained coherent. Comparison with published data fov pure nickel showed that aluminum greatly re-tavded softening and recrystallization, but it made little difference whether or not particles were present. The presence of pakticles led to a heterogeneous distribution of precipitates after annealing at 700" to 750°C. Recovery was not detected. Recrystallization occurred by the growth of new grains into unrecrys-tallized material. In a previous study by the author,&apos; the growth of Ll2-type ordered yl(Ni3Al) precipitates was followed in Ni-12.7 at. pct A1 alloy as a function of aging at 600" and 700°C. The particles were showo to be cubical in shape in all sizes from 50 to 3000A and remained coherent. This work was used as a guide in preparing the starting structures for the present study of the effect of these particles on the annealing behavior of heavily cold-rolled strip. Another question of present interest was whether dislocation and particle hardening were additive, since the structures before rolling ranged from solution-treated to peak-aged to overaged. Also, precipitation might occur on annealing after cold-rolling. Reference may be made to other papers2"5 for previous work in this relatively unexplored field and only some recent work will be mentioned her:. phillips2 studied the effect of deformable 0 to 590A-diam cobalt particles on a Cu-3.23 pct Co alloy rolled 95 pct and found that the particles, which rolled out into thin lamellae, impeded softening and recrystallization. Tanner and servi3 likewise studied the annealing of cold-swaged Cu-2 pct Co alloy containing 150A-diam particles and found impeding effects. Haessner et a1.,4 on the other hand, found that incoherent 2-p-diam non-deformable particles of B4C (0.04 vol pct) tended to increase the rate of recrystallization of copper rolled up to 95 pct reduction. They attributed this to the formation of new grains at the particle interfaces. Humphreys and artin&apos; found that nondeformable silica particles in copper rolled to 30 pct reduction accelerated recrystallization if the particle spacing was large and retarded it if the spacing was smaller. Haessner et a1 4 also studied a rolled Ni-Cr-A1 alloy; however, the particles of y&apos;(Ni3Al)-type precipitate were not put in before rolling, but separated during the isothermal annealing at 750°C. No previous work appears to have been carried out on the effect of y&apos; (Ni3A1) particles on the annealing of Ni-A1 alloy. Hornbogen and ICreye7 redetermined the solubility c of aluminum in nickel as a function of temperature T and showed that it was given by c = 32.6 exp(-1940/RT). This relation gives aluminum solubilities of 15.1, 14.2, 12.0, and 10.7 at. pct at 1000°, 900°, 700°, and 600°C, respectively. The phase precipitated from the nickel-rich solid solution is fcc y1 (Ni3A1) which has a Cu3Au -type ordered structure8 and remains ordered up to 1000°C.B EXPERIMENTAL PROCEDURE The alloy used was identical with that used before. Chemical analysis showed 6.27 wt pct (12.71 at. pct) Al, the principle impurities being 0.065 pct Fe, 0.022 pct Co, 0.020 pct Cu, and 0.004 pct C. Bar stock of 1 in. diam was cold-swaged to % in. diam, cold-rolled to 0.300-in.-thick strip, and annealed at 900°C in dry hydrogen. It was cold-rolled to 0.100-in. thickness and solution-treated for 1 hr at 1000°C while sealed in a quartz tube in argon, quenching in iced brine with the aid of a device to snap off the nose of the tube. Lineal analysis gave an average grain size of 0.055 mm. Pieces of strip were aged at 700°C in vacuo for 30 min, 51/4 hr, and 1 week to produce nominal average particle widths of 60, 150, and 500A, respectively, as known from the previous work.&apos; The average diamond pyramid hardness was determined. The heat-treated strips were rolled from 0.100 to 0.005 in., a reduction of 95 pct, and the rolled strips stored at about -5°C. Small pieces were annealed within 1 week for 30 min at temperatures from 300° to 950° ±2°C in a horizontal vacuum furnace. Strips were withdrawn into a cooling zone, giving an estimated initial cooling rate from 950°C of about 50°C per sec. Average diamond pyramid hardnesses were determined on a lightly electropolished spot on the surface of each strip using 300-g load. Each point on the softening curves represents a separate annealed specimen. Sections containing the rolling direction were examined by optical metallography. Selected specimens were electrothinned to the center plane&apos; and examined by transmission at 100 kv in a Siemens Elmiskop I electron microscope. It is well-known that changes in the structure tend to occur when a deformed strip is electrothinned below a thickness of a few hundred angstroms, although this is less serious with a material such as nickel which has a high melting point, and also is apt to be less serious when particles are present. Observations were nevertheless confined to thicker regions of the foils with estimated thicknesses over 1000A. No changes were observed due to beam exposure.

Jan 1, 1968