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By P. Greenfield, C. C. Smith, A. M. Taylor

J. E. Harris (Berkeley Nucclear Laboratories, England)—Greenfield et al.11 attribute abrupt changes in slope of their log o/log i curves for heat-treated Mg/0.5 pet Zr alloy (zA) to &apos;atmosphere&apos; locking. It is proposed here that a more reasonable explanation of the apparent strengthening at low rates of strain can be based on precipitation either during the preanneal or during the creep tests. All the tests were carried out above 0.5 Tm where solute atmospheres are likely to be largely evaporated2 and can migrate sufficiently rapidly so as not to impose any &apos;drag&apos; on the moving dislocations. McLean3 has derived an expression for determining the temperature Tc above which, due to the high-migration rate of the atmospheres, Cottrell or Suzuki locking can play no part in determining creep strength. This expression, which holds for an applied shear stress of not greater than 5 X 107 dynes per sq cm is: Tc/Tm= 7/6.8 - log10? where i = secondary creep rate The values for T, corresponding to the maximum and minimum reported creep rates at each temperature have been calculated from the data of Greenfield et al. These are given in Table VII. All the test temperatures were above T,, the margin being greater for the higher temperatures and for the lower strain rates where the breaks in the log s/log ? curves occurred. Dorn and his collaborators14, 17 have studied systematically the effect of solute hardening on the creep properties of an A1/3.2 at. pet Mg alloy. In the temperature range where strain aging occurred in tensile tests, abnormally high-activation energies for secondary creep were obtained but at temperatures above 0.43 Tm, solute alloying did not have any effect on the creep parameters. Moreover, there have been no reports of any strain aging phenomenon during elevated temperature tensile tests with ZA material.18 Instead of the observed strengthening being due to atmosphere locking, it is now proposed that precipitates play an important role in enhancing the creep strength of the material. There are two possibilities—precipitation of zirconium hydride during the high-temperature preanneal and/or precipitation of the hydride or a-zirconium during creep. On the basis of the former the results can be interpreted in terms of a critical stress being necessary to force the dislocations through or over preexisting precipitates. From the latter, if the strengthening is due to pre- cipitation during the test then hardening should be associated with a critical strain rate. At low rates of strain, time is available during the tests for precipitation to occur either directly onto dislocations (thus pinning them) or generally throughout the matrix (which would impede dislocation movements). Examination of the data of Greenfield et al. suggests that both mechanisms may be operative since they observed precipitation during creep and also found that their alloys exhibited high-creep strength in the early stages of the low-stress tests, i.e., before creep-induced precipitation had time to occur. It is not easy to understand why they considered that precipitation of zirconium hydride is unlikely to occur at 600°C while it can take place in tests in air at as low a temperature as 200°C. Precipitation of the hydride during the preanneal cannot be ruled out merely on the basis of metallographic examination. Hydride precipitates in ZA type alloys are very small and can only be accurately resolved in the electron microscope.9 For example, in this laboratory20 hydride platelets with major dimensions <(1/10) µ have been observed by electron transmission through thin film specimens of hy-drogenated ZA material. Complex interactions between dislocations and such particles are illustrated in Fig. 12. Additional evidence for precipitation during pre-annealing is provided by the data presented in Greenfield&apos;s Fig. 1 and Table IT. These show that the creep strength at 200o and 400°C increases with the time of preanneal at 600°C. Such increases cannot be explained on the basis of increases in grain size alone for further improvements in strength were observed when the material was annealed for longer times than that required to stabilize the grains. Although the main discussion is confined to ZA material, similar arguments can be used against the strain aging hypothesis proposed to explain the binary Mg/Mn alloy data. In this case no precipitation is possible during the preanneal, but precipitation-hardening during creep can occur.

Jan 1, 1962

Early theories of coal formation are outlined, with special emphasis on the arguments for allochthony and autochthony. Various aspects of the nature, growth, and decay of the characteristic vegetation of the brown coal peat moors, their conversion into coal, the origin of banding, and the influence of tectonics are discussed.A description of the banding in Victorian brown coals is followed by a discussion of their vitrain, fusain, and natural carbonized coal; and concludes with the nature of the coal resin and the possibilities of its extraction.The nature and derivation of inorganic matter in brown coal, based on Lessing&apos;s classification, is described. Assimilation of mineral substances in specific plants with variations due to environmental factorsare illustrated by analyses of present day trees. Consideration is then given to possible sources of salt, marcasite, and quartz in brown coal.It is shown that part of the inherent and extraneous ash may have been removed during and after coal formation. The nature and abundance of the organically combined substances in brown coal emphasizes the anomalies that may arise from estimating the total inorganic matter from ash contents.After classifying deposits on external heating surfaces of boilers, theoretical and practical aspects of slag formation, alkali matrix deposits, and the effect of sulphur and chlorine are considered.Analyses of deposits in boilers burning Victorian brown coal are tabulated.Slagging at the Yallourn power station from sand in the Yallourn open cut, and difficulties with Yallourn North Extension coal at the Maryvale paper mills are described.Tests carried out on Morwell and Yallourn coals showed that with the former, impacted deposits formed on boiler heating surfaces, and left a high percentage of chlorides on probes. Morwell briquettescompared with Yallourn briquettes also reduced the running time of a semi-industrial boiler through deposits with sodium sulphate as...

Jan 1, 1962

By L. Adler

Some estimate of the geologic pressures existine at the site of a proposed underground opening is essential for its economic design and construction. Regardless of the size of such an opening, drill hole, or mine stope, these primitive stresses need evaluation; at present a number of techniques are available for this purpose. However, a new method of analysind stresses is proposed in this paper. Some estimate of the geologic pressures existing at the site of a proposed underground opening is essential for its economic design and construction. Regardless of the size of such an opening, drill hole or mine stope, these primitive stresses need evaluation. At present a number of techniques are available for this purpose, and another one is to be proposed. These may be grouped into three general methods: 1) precedent, 2) instrumentation, and 3) theoretical analysis. The first two are covered in the literature where their advantages, as well as limitations, are discussed.&apos;9&apos; Generally a theoretical approach combines structural geology with engineering mechanics. The former deals with the geodynamic causes of residual stresses (stresses not related to overburden weight) and presents interesting, but controversial, views.&apos;" A general and useful conclusion, however, can be drawn - vertical residual stresses are much less prevalent than horizontal. However, if for some reason, the values and effects of horizontal pressures were better known to engineers the following analysis

Jan 1, 1962

By W. C. Hagel, J. H. Westbrook

Usittg a sectioning technique with Agl10 as the tracer, the diffusion of silver in silver-excess (45.8 at. pct Mg), near-stoichiometric (49.8 at. pct Mg), and magnesium-excess (52.0 at. pct Mg) cylinders of CsCl-type AgMg was determined from 500" to 700°C. Diffusion coefficients conform to the expression D = Do exp (-q/RT) where the respective Do values are 1.53, 0.280, and 0.134 sq cm sec-I and the Q values are 41.3, 40.6, and 38.0 kcal g-atom-&apos;. Lnttice-parameter and density measurements were performed on a more numerous assortment and wider range of compositions. Substitutional defects were found on both sides of stoichiometry. Activation energies for other rate processes in these alloys show related trends with changing composition, although silver may not be the rate-detemining species. KNOWLEDGE of diffusion coefficients is necessary for a quantitative understanding of the many rate processes (e.g., grain growth, precipitation, sintering, oxidation, or mechanical deformation) occurring in solids. Although these data are available for most metals and common alloys, they are quite limited for intermetallic compounds—a group of materials whose unique physical and mechanical properties are presently attracting great interest. From a fundamental viewpoint, diffusion in intermetallic compounds also offers several engaging aspects owing to: their ordering, the possibility of introducing large, stable concentrations of lattice defects, and the variety of bonding types and crystal structures which can be found. In the case of CsC1-type compounds, some previous work has been directed at examining the role of vacancy defects by changing their concentration compositionally. The diffusion of Co60 was measured in 0 NiAl1- and in P COA., Except for the results of Smoluchowski and Burgess, isothermal diffusion coefficients were found to pass through a minimum at the stoichiometric composi- they decreased sharply on what was reported by Bradley and co-wrkers&apos; to be the vacancy-rich (aluminum excess) side of stoichiometry. This investigation of the diffusion of Agl110 in AgMg was undertaken both as an adjunct to a concurrent study of its deformation behavior and for the purpose of obtaining information on the influence of lattice defects and temperature on diffusion in another CsC1-type intermetallic compound. Bcc AgMg remains ordered up to and melts congruently at 820°C. Solubility limits at 300°C are about 41 at. pct Mg and 53 at. pct Mg. It is one of the Hume-Rothery electron compounds with a 3/2 electron-atom ratio. Previous investigations of its properties include hardress,&apos; tenile,&apos;-&apos; electrical reistivity, and thermodyna-mic1&apos;,14 studies. Indications of a high bonding strength may be found in the large heat of mixing1&apos; and in the 6-pct vol contraction on compound formaticp, as calculated using atomic radii of l.40 and l.55a for Ag and Mg. EXPERIMENTAL PROCEDURE Alloys were prepared by the induction melting of selected fine silver (99.95) and low-iron magnesium (99.95) in magnesia crucibles under 1 atm of A. Supplied by the Handy and Harmon and Dow Chemical Cos., respectivelv. Melts were poured under argon into graphite molds providing 1 1/8-in.-diarn. by 4-in.-long ingots. These were homogenized in evacuated and argon-filled fused-silica capsules by heating for 16 hr at 750&apos;. Three 1 in.-diam. by 3/4-in.-long cylinders were machined from the mid-portion of each ingot for diffusion measurements. Three alloys, analyzing 45.8, 49.8, and 52.0 at. pct Mg were taken as representing the extremes of interest, with 49.8 at. pct Mg being very close to the stoichiometric composition of 50.0 at. pct Mg.

Jan 1, 1962

By Hsun Hu

Three single crystal strips of a 3 pct Si-Fe alloy with approximately (110) [001], (210) [001], and (100) [001] orientations were rolled at room temperature to 30, 50, and 70 pct reductions in thickness. Their deformation and annealing textures were studied. In most cases, the change in texture upon recrystallization and subsequent growth can be described as rotations around the <I10 > axes. A < WO > rotational relationship was also observed. The temperature dependence of recrystallization textures was discussed. WhILE considerable data have been published on the rolling and annealing textures in silicon-iron crystals, very little study has been made on the texture formation at various stages of rolling deformation, and during the process of recrystallization. Dunn&apos; in some of his early works had studied the orientation of recrystallized grains in crystals cut out from lightly rolled (10 to 20 pct reduction) large grained sheets. He found that in most cases a third-order twin relationship exists between the crystal and the recrystallized grains. This orientation relationship actually corresponds to rotations around the <110> axes. The more recent studies of Dunn &apos; and of Dunn and Koh &apos;5 on the rolling and annealing textures in various silicon-iron crystals were concerned mostly with a cold-rolling reduction of 70 pct and annealing at 980OC for recrystallization. Reductions of similar magnitude were also employed by Walter and Hibbard in rolling columnar crystal aggregates of a silicon-iron ingot. A systematic study of the effect of rolling reduction on the deforma- tion and annealing textures is still lacking. Regarding the effect of annealing temperature on the texture formation, Dunn3 has observed a change in therecrys-tallization texture by annealing a 70 pct rolled (1 10) [001] crystal first at a low temperature then atahigh temperature. But the details of texture formation during the annealing treatments were not thoroughly investigated. The present investigation was undertaken to study the texture developments at various stages of rolling deformation and of the recrystallization process, so that a better understanding on the texture formation in silicon-iron crystals may be obtained. EXPERIMENTAL PROCEDURE The three single crystals used in the present investigation were selected from the group of single crystal strips previously prepared7 from a high grade commercial Si-Fe alloy with 3 pct Si. The thickness of these single crystal strips was 0.040 in. The orientations of the three crystals as determined by the X-ray back-reflection Laue technique are shown in Table I. Each of the three crystals was rolled at room temperature along the strip direction to 30, 50, and 70

Jan 1, 1962

By Julian Glasser

Starting with rutile, containing more than 55% TiO2 and of the proper particle size, the commercial production of titanium tetrachloride via fluidized bed chlorination is relatively very simple and economical. As compared to shaft chlorination, it operates at a much higher capacity for given sizing of equipment, and appears more foolproof, requiring less attention. Operating data were obtained on a 53" diameter fluidized bed chlorinator using Australian rutile and petroleum coke of controlled particle size. Production rates varied from 20 to 50 tons of crude TIC14 per day for a campaign extending over one month. Close to theoretical yields and efficiencies were obtained from the viewpoint of chlorine and/or rutile consumption. Details of important equipment design, critical operating conditions and pertinent results are described.

Jan 1, 1962

By G. M. Schwartz, J. N. Gundersen

John W. Gruner (Professor Emeritus, College of Science, Literature, and the Arts, Dept. of Geology, University of Minnesota, Minneapolis) — It is surprising that two men as well acquainted with the taconite rocks of the Mesabi District as Drs. J. N. Gundersen and G. M. Schwartz should have concluded that the taconite of the Eastern Mesabi before the intrusion of the Duluth gabbro consisted largely of quartz and magnetite. These minerals were "locally reconstituted" into "a wide variety of silicate mineral assemblages" by the gabbro. It is well known, of course, that the silicate mineralogy of the Eastern Mesabi (&apos;about 14 miles in length) is quite different from that of the Main Mesabi which is over 60 miles long. The change from one to the other is abrupt and cannot be attributed to any other cause than the thermal effects of the gabbro. Are we to assume or believe that the taconite of the Eastern Mesabi was radically different from that of the Main range before the gabbro metamorphosed it?

Jan 1, 1962

By C. H. Li, R. J. Stokes, T. L. Johnson

The effect of alumina particles on the nucleation and growth of cracks through a silver- chloride matrzx has been investigated. It has been found possible to promote fibrous cracking in dispersion-strengthened silver, chloride under notch-impact conditions at temperatures at which silver chloride alone cleaves brittlely The modification) of fracture beIzavzor is thought to be due to the relaxation of hydrostatrc stress beneath a notch by the nucleation of cavities near alumina particles. In recent years, composite or dispersion-strengthened materials have been studied primarily to understand their high resistance to plastic flow particularly at elevated temperatures. Dislocation models have been developed with which it is possible to deduce with fair success the effects of interparticle distance, particle size, temperature, upon yielding and creep behavior.l-4 Much less attention has been paid to the fracture behavior of these materials (with the notable exception of common structural steels) and little is known experimentally about the manner in which inclusions affect the nucleation and growth of cracks through a matrix. Nevertheless a beginning has been made in connection with fibrous cracking in ductile matrices where inclusions appear to play an essential ro1e.5-7 During the severe localized plastic deformation which accompanies necking in a tensile test, cavities are believed to develop at inclusions; these cavities subsequently grow and coalesce by plastic flow until separation is complete. It is of interest to consider whether inclusions can affect fracture behavior under loading conditions which restrict the plasticity of the matrix itself (for example, cleavage under conditions of a high imposed strain rate at low temperatures). It is particularly interesting to study these effects in a solid which shows a spectrum of behavior ranging from fully ductile to semi-brittle behavior. Such a solid is silver chloride whose mechanical behavior depends sensitively upon temperature and strain rate.&apos;," The present paper is concerned with a study of the influence of inclusions (in the form of alumina particles) on the fracture behavior of silver chloride loaded uniaxially at low strain rates at room temper- ature and also under notch impact conditions over a wide range of temperature. In particular, it will be shown that the alumina particles can exert a startling effect on the ductile-brittle transition temperature of notched silver chloride and that the magnitude and nature of the effect depends upon both the quantity of alumina and the shape of the alumina particles. 1. EXPERIMENTAL PROCEDURE 1.1 Materials Used. Silver chloride powder of analytical reagent (AR) quality having an average particle size 6 was supplied by the Mallinckrodt Chemical Works (st. Louis, MO.). Acid washed 900 mesh alumina powder, designated A38-900, was supplied by the Norton Co. (Cambridge, Mass.). This powder was added to silver chloride in two forms: a) the as-received condition in which the individual particles were of random irregular shape; their statistical average size was 7; b) in a condition in which each particle was spherically shaped by a fusion technique. In this case, the statistical average particle size determined with the optical microscope was approximately the same (about 5p) but electron micrographic evidence indicated that many ultra fine particles were present in the spheroidized powder. 1.2 Preparation of Composite Materials. Silver chloride-alumina composites containing 2.5, 5, and 15 pct by volume of alumina were produced by the extrusion of mechanically mixed powders blended in a ball mill for 24 hr at room temperature. The mixtures were compacted at 50,000 psi at room temperature in the form of billets 3/4 in. in diameter and 1 in. long which were then extruded with a 16:l reduction ratio at 370°C through a radius-type steel die having a 5 deg lead-in angle. An extrusion temperature of 370°C was selected to ensure that all composites had sufficient plasticity to be extruded. Apart from this general requirement, the choice was arbitrary. 1.3 Microstructure of Composites. Attempts were made to check the distribution of alumina metallo-graphically by polishing transverse and longitudinal sections of the extruded rod. Specimens were wet-ground to 600 emery paper and lapped successively with 5 and 0.25-p grades of diamond paste. They were etched for 10 sec in 10 pct sodium thiosulfate solution and lightly polished in concentrated ammonium hydroxide. The most effective way to render the alumina particles and grain boundaries visible was to radiate the surface with intense white light to decorate the grain boundaries and the particle-matrix interfaces photolytically.

Jan 1, 1962

By T. C. Shelton, W. M. Huang

One of the problems arising from the use of modern machines and systems in coal mining is increased emission of explosive gases into the mine passageways. Interest in degasification of coal seams has grown. The authors summarize the results of coal permeability tests done at Virginia Polytechnic Inst. on one of the fundamental aspects of the problem. There are undoubtedly many factors that affect the emission of gas from coal but the permeability of coal to gas flow would seem to be fundamental. However, there is very little information on coal permeability to gas flow available in the U.S. at the present time, despite the fact that such knowledge would appear to be significant in any degasification effort. Studies made recently in the mining engineering laboratories at Virginia Polytechnic Inst. have determined values of permeability on 1-in. cubes of selected coals. COAL PERMEABILITY The permeability values given in this paper are based on adaptations of Darcy&apos;s law formulated by Henry Darcy in I856 from experiments with fluid flow in porous media.&apos; Using air as the gaseous fluid, they were obtained by employing similar methods as are used to dete1:mine the permeability of petroleum and gas reservoir rock specimens. Permeability is. a measure of the ease with which fluids flow through a porous substance, and it is governed by the connected pores within a porous medium. If a few large-sized pores, fractures or channels are present within the medium, the medium can have great permcnability without significant porosity. It is reasonable to assume, therefore, that the permeability of coal, due to its structure, is based on fractures connecting the pore space left as the result of some degree of devolatilization or other changes of the substance from which coal was formed. The results of this irvestigation tend to validate this assumption in that the values obtained indicate a close relationship between the rank and permeability of coal. COALS TESTED AND PROCEDURE The coals whose permeability values were determined in this investigation are given in Table I.

Jan 1, 1962

By I. F. Jackson, H. L. Hartman

Hard-metal inserts have received considerable attention in the mining industry recently for a variety of excavating and penetrating purposes. Their use in percussive drilling and in coal cutting machines is well known, but attempts to utilize them in cutting materials such as dimension stone have been discouraging because of excessive tool wear and failure. Particular attention is given to those properties of hard-metal inserts that affect their resistance to wear. A consideration of the actual wear mechanism shows the importance of correct mounting of the inserts and of the selection of suitably powered driving motor so as to achieve minimum tool wear and maximum tool life. Comparisons are made between the performances of types of hard-metal inserts, relating their inherent properties with results obtained in laboratory tests. As part of a broad program to improve the quarrying and processing of industrial minerals, The Pennsylvania State University has been investigating the machinability of slate under laboratory and field conditions. It should be emphasized that the results of the research presented in this paper are also applicable to other natural structural materials, and particularly to the more workable ones such as limestone and sandstone. Improvements which accrue in cutting and sawing should prove of benefit to all the dimension stone industry. Further, it may be pointed out that the results reported here are applicable to rotary drilling (with drag bits) as well as to cutting and sawing of rock. INVESTIGATIONS IN RELATED FIELDS The investigation was initiated with an extensive survey of available literature related to metal cutting and to rotary drilling. The following similar features between metal cutting and slate cutting became evident: 1) Hard-metal inserts are widely used as a cutting tool in both cases. 2) The forces acting on the tool may be resolved into normal and tangential components. 3) Rate of penetration and tool wear are important criteria in each case. On the other hand, important differences also exist: 1) Most metals, exhibit plastic behavior, while slate (and most rock) is a brittle material under normal conditions. 2) In metal cutting the component of force acting parallel to the surface of the workpiece is considerably greater than the force holding the tool against the workpiece. 111 slate cutting, this situation is reversed. Similarities between drag-bit rotary drilling and slate cutting are as follows: 1) In both casts, a tool, usually of the hard-metal insert type, is used to penetrate a brittle material. 2) The drilling forces and related variables, such as rotation speed, are similar. 3) Chip formation in each case is essentially the same. 4) The shape of the tool is similar in rotary drilling and slate cutting. Important differences are also apparent: 1) The objective of drilling is to produce a directed hole, while in cutting it is to form a kerf. In core drilling, however, a kerf is also produced. 2) The horizonta1 component of force in rotary drilling decreases from the center to the outside of the tool, whereas in slate cutting the component is almost uniformly distributed across the width of the tool. 3) The power absorbed in the drill rod is greater in rotary drilling. 4) The clogging action of chips, if excessive power is applied to the tool and if flushing is insufficient, is more serious in rotary drilling. Because of the striking similarities between metal cutting and slate cutting, and between rotary drilling and slate cutting, it was considered that the findings of investigators in those fields would serve as a guide for experimental studies of slate cutting. The following is thus devoted to a discussion of those aspects of metal cutting and rotary drilling pertinent to the present investigations.

Jan 1, 1962

By John Rogers

The goal of a detailed quantitative understanding of the variables insulfide flotation in terms of established, or new, scientific principles is still distant, although there has been a good beginning in the past 50 years with more rapid progress since 1930. Advances have paralleled closely those in other branches of surface chemistry and the development of a series of experimental techniques such as contact angle, surface area measurement, radioactive tracers, infrared spectra, electron diffraction, monolayer, and electro- chemical methods of investigation. The second editions of books by Sutherland and Warkl ( 1955) and Gaudin2 ( 19571, are detailed accounts of this progress. The complexity of sulfide mineral flotation systems is indicated by Sutherland and Warkl who list 32 variables of flotation, of which only 22 can usually be controlled by the metallurgist. A consequence of this multiplicity of variables, many of which may be specific to each particular ore, is that ways of floating sulfide minerals from new ores are still developed empirically. How- ever, this review will try to show how the chemistry of the function of frothers, collectors, depressants, and activators in sulfide flotation is being steadily unravelled. Chiefly, it will be concerned with the interaction of pure soluble compounds with individual sulfide minerals, the surfaces of which are often not stoichiometric for several reasons discussed by Plaksin.3 As a result, for example, a freshly cleaved galena surface has cathodic and anodic areas which have different degrees of oxidation and different reactivity to- wards collectors like xanthate. Such complicating considerations should be remembered in the subsequent discussion of pure minerals. THE NEED FOR FLOTATION REAGENTS After considerable controversy it has been established with a few exceptions that unoxidized, uncontaminated sulfides will not float. Moreover all flotation plants recovering sulfide minerals use collectors which are removed from the circuit with the sulfides. Gaudin, Miaw, and Spedden4 have discussed the relation between the crystal structure of solids and the native floatability of the exceptions mentioned above. A second question which has been much explored is the nature of the surface on which a collector like xanthate is adsorbed or reacts. Is this the un- changed surface of the sulfide mineral, or does the adsorption depend on the initial oxidation of the sulfide surface ? Sutherland and Warkl and Gaudin2 discuss the work of Taggart5 and others on this question without reaching any other conclusion than that oxygen was important.

Jan 1, 1962

Extensive geophysical exploration and drilling operations have been: conducted in, South Central Queensland by Phillips Petroleum Company and Sunray DX Oil Company since late 1959. The main outlines of subsurface geology are now known, but many problems must be solved before a comprehen sine. picture can be presented of the geology and petroleum prospects e Interpretations to date suggest that -fiddle Paleozoic sedimentary rocks, probably, related to the Tasman belt of geosynclines, once extended. over. most. of the area An oro;eny 2.n late Paleozoic time, succeeded by deep pre-Pexmian erosion, removed the older sediments over large. areas, but Paleozoic sediments, were preserved from erosion in the Adavale and ancillary structur-a.l basins. Marine sediments of Devonian age are con-sidered prospective source beds for petroleum. Current work is directed toward finding favorable structure and reservoir beds to test the oil prospects of the area.

Jan 1, 1962

By J. W. Montoya

The chemical, mineralogical, and physical properties of berylliferous tuff from Spor Mountain, Utah, were determined in laboratory research conducted by the Bureau of Mines. Two beryllium-bearing minerals--a hydrated form of bertrandite and a berylliferous saponite--were found to be present in the tuff. Each of the beryllium mineral forms predominated in samples from certain areas of the district. The possibility of practicably separating the beryllium minerals from the tuff by physical methods appears remote because of the complexity and nature of the mineral associations. Beryllium mineralization in the region occurs in a rhyolitic tuff usually overlaid by unaltered rhyolite. The beryllium is distributed erratically throughout the tuff in individual mineralized bodies. Many samples of mineralized tuff were examined and found to contain from 0.2 to 1.8 percent BeO. All samples contained a hydrated form of bertrandite that was nearly cryptocrystalline, whereas samples from one area also contained a berylliferous saponite of variable beryllium content. Neither mineral has been previously reported, although related bertrandite-like minerals have been found in the U.S.S.R. and berylliferous minerals of the montmorillonite group have been synthesized. Most of the minerals of the tuff are finely crystalline, intergrown, and have similar densities. The complexity and intimacy of the mineral associations, the difficulty of achieving effective mineral liberation, and the highly friable nature are characteristics that lead to the conviction that tuff of the type examined cannot be effectively concentrated by gravity, magnetic, electrostatic, attrition, washing, sizing, or flotation methods.

Jan 1, 1962

By E. T. Turkdogan

This is a compilation and a critical review of the data on the Fe-Ca-0 ternary system. Using the results on the reductiorz-equilibria, an oxygen potential diagram is drawn for the greater part of the system. A number of univariant systems and invariant points, not determined experimentally, are evaluated by making use of the theorem on univariant curves intersecting at an invariant point. The formation of solid solutions and ternary compounds and the crystal structures of some of the phases in the composition-diagram are given for a feu! temperatures. DURING the past thirty years there has been a continued interest in the study of the Fe-Ca-0 system. A detailed literature survey made by white1 in 1943 indicated that further work was required to clarify the phase relationships; in fact, the work carried out in the subsequent years, reviewed by Burdese2 in 1954, made a valuable contribution to a better understanding of this subject. Most of the data were obtained by the step-wise reduction of mixtures of iron oxides and calcium ferrites. However, there is some uncertainty about the phase relationships in this system, arising mainly from insufficient use of thermodynamic concepts in the construction of phase diagrams. In this paper an attempt is made to establish the invariant points from the available data. OXYGEN POTENTIAL DIAGRAM Schenck and coworkers3,4 were the early investigators who studied part of this system by the step- wise reduction method and suggested the formation of two ternary compounds, CaO.FeO.Fe2O3 and 2Ca0.5Fe0.2Fez03, the latter being referred to as point X. They also deduced from their results that the phases Y (8.74Ca0.32.5Fe0.8.74Fe2O3 and Z (2.02CaO-97.98FeO) were formed near the w?stite corner of the system. Martin and voge15 postulated the existence of the compounds CaO.9FeO and 4Ca0.3Fe3O4; the former is very close to the composition of point Z and the latter to that of CaO.FeO-Fe2O3. The most valuable contribution to the presen knowledge on this system was made by Cirilli and Burdese6-8 who showed by X-ray and chemical anal yses that there were two ternary compounds, CaO-Fe0.Fe2O3 and CaO.3FeO-FezO3; the former is the same as that suggested by Schenck et al. and the latter is close to their point X. The results of Cirilli and Burdese show that the phases Y and Z postulated by Schenk et al. are solid solutions of calcium oxide in w?stite. In most of the above-mentioned reduction-equilibria measurements carbon monoxide-carbon dioxide mixtures were used and in a few cases hydrogen-water vapor mixtures were employed. Using the

Jan 1, 1962

By Roland F. Beers

At East Union, Knox County, Maine, near the shore of Crawford Pond, an outcrop of basic rock has been known for more than a century. The occurrence has been regarded as an unusual type of peridotite-pyroxenite, containing disseminated and massive pyrrhotite with nickel, copper and cobalt in recoverable amounts. From the outcrop, the sulfide body had been mapped more or less continuously for a distance of two miles through geophysical methods of several kinds. This paper describes the methods in sufficient detail to evaluate their significance. A core drilling program has con- firmed the location of the conductor and offers a positive means of correlating the geophysical measurements with the physical properties of the ore body. The history of the exploration offers a unique opportunity to evaluate the method of multiple geophysical methods.

Jan 1, 1962

By E. Eichen, G. S. Ansell. L. R. Sefton

A Technique for the Preparation of Thin Films of Two-Phase Alloys Suitable for Use in Transmission Electron Microscopy In order to obtain foil sufficiently thin to permit transmission electron microscopy of two-phase alloys, particularly alloys in which the second phase is present as a very finely dispersed second phase, a technique has been developed to permit the thinning of these materials without either the large degree of pitting present in the electrochemical or chemical thinning process or the slicing of the second phase particles accompanying the mi-crotoming process. The metal or alloy to be thinned is first ground to initial sheet thickness of approximately 0.002 in. by hand grinding on 4/0 emery paper. This starting sheet of material is then reduced in cross section by an air-abrasion technique using an S. S. White dental abrasive unit. This unit consists of a supply of compressed CO, which provides a stream of high velocity gas impinging on the metal surface. Incorporated in the machine is a hopper-type of device in which fine abrasive particles of alumina are introduced into this high velocity gas stream. The abrasive particles are irregular in shape, approximately 30 across. If any particles are introduced into the sample during thinning, they should be readily observable. Impingement of this gas abrasive mixture on the metal surface causes rapid removal of the metal in a rather uniform manner. The rates of metal removal may be adjusted by both regulating the gas pressure and amount of abrasive material introduced into the gas stream. By moving the gas stream abrasive mixture slowly about the specimen or sheet surface, a large area of the sheet may be uniformly reduced to a thickness which is then suitable for use in transmission electron microscopy. Attendant with this metal removal is a result in cold working of the metal surface due to the impingement of the abrasive particles. The resultant foils, therefore, if made from materials which are desirable to view in the annealed condition, have to be subsequently heat treated. If the alloy from which these foils have been made has been initially heavily worked or deformed during manufacture, then no subsequent heat treatment is, necessary as in the case of the SAP-type alloys. Following this initial abrasive thinning technique, the material is then given a final electropolish which is just sufficient to remove any oxide which has formed on the metal surface during the abrasion technique. Care has to be exercised in this technique to make sure that none of the attendant problems associated with the chemical or electrochemical removal process are encountered. An electrolyte solution which has been found suitable for aluminum-aluminum oxide SAP materials is one containing 78 ml of perchloric acid, 120 ml of distilled water, 700 ml of ethanol, and 100 ml of butylcellosolve. The current density used is 1 amp per sq cm and a polishing time of 3 sec on each side of the foil is used. Extreme care must be used in choosing the current density and time to ensure that just the oxide film on the specimen is removed. Times or current density which are greater than this will lead to perforation of the film due to the removal of the A1,0, particles or a complete loss of the film due to complete solution of the matrix. Once the oxide film is removed the specimens must be kept in alcohol until placed in the microscope to prevent any further oxidation. Fig. 1 shows -an electron micrograph at X28,000 of a thin foil of an aluminum-aluminum oxide SAP-type alloy prepared using this technique. The alloy consists of a matrix of commercial purity aluminum containing a very finely dispersed second phase of aluminum oxide flakes. In the electron micrograph, the dark patches are the aluminum oxide particles. The lighter portions of the micrograph are the aluminum matrix. Within the aluminum matrix, the dislocation structure of the alloy is clearly visible. This structure consists of intersecting twin boundaries and single dislocations. No abrasive particles were observed in the samples. In addition, thin films of commercial purity aluminum were prepared using this method and observed in the electron microscope. Here also, there was no evidence of abrasive particles introduced in the samples. The technique presented provides a satisfactory method for the production of thin films of aluminum-aluminum oxide SAP-type alloys for use in transmission electron microscopy where none of the usual thinning techniques appears to be satisfactory.

Jan 1, 1962

By Tennyson Smith

Jan 1, 1962

By I. R. Kramer, L. J. Demer

T. H. Alden and R. L. Fleischer (General Electric Research Laboratory)— The authors&apos; results indicate clearly and, we believe, significantly that during tensile deformation the surface layers of an aluminum crystal are hardened more severely than the interior of the crystal. A probable explanation of this effect, as the authors indicate, is that dislocations in the primary slip system may be obstructed at the surface or, it should be added, near the surface. The intent of this discussion is to show that the oxide film on aluminum is not likely to be responsible for this effect, but that the results can be understood if it is assumed the secondary slip is more active in the surface layers than in the interior. Prior study has shown that the principal mechanical effect of an oxide film on a single crystal is to raise the yield stress while leaving the rate of strain hardening during the initial deformation relatively unaffected.33 Since the yield stress is unchanged during polishing in the present case, we conclude that continual removal of the oxide film exerts a small effect on the plastic hardening.* It appears that the hardening interactions are occurring not only at the immediate surface, but to an appreciable depth below it, although with decreasing severity. For example, Kramer and Demer found that with removal of 0.004 in. from a specimen, the easy glide region was extended somewhat; but the yield stress did not decrease. The initial yield stress was recovered only after 0.041 in. was removed. Since a very brief polish would permit dislocations trapped behind a surface film to run out,34 extra dislocations must, instead, be trapped to a considerable depth below the surface. The same conclusion is drawn from the observation of decreasing hardening slope with increasing surface removal rates. If the hardening interactions were only at the immediate surface, a full softening effect would be observed at some small removal rate. The view is taken here that strain hardening is principally caused by small amounts of secondary slip.35 The secondary dislocations will interact in various ways with the primaries, interfering with their motion and causing them to accumulate in the crystal. Prior studies of easy glide have shown Diehl&apos;s model of hardening to be qualitatively consistent with the effects of impurities,36 of temperature,36 and of crystal size.37 On this basis the enhanced hardening of the surface layers in aluminum arises from increased secondary slip at and to some depth below the surface. Selective removal of this hardened layer is expected to decrease the measurable "bulk" hardening, the effect increasing with the removal rate and decreasing with the applied strain rate. We suggest that the stress on secondary systems is raised by the bending moments arising from interactions with the grips during the deformation. This stress from the grips has been shown to be a maximum37 near the surface, and hence, increased secondary slip should result. Prior investigations of grip effect:; indicate that as the grip stresses are raised by changing the crystal shape, the easy glide slope increases while the extent of easy glide decreases.38-40 It has been shown also that bending moments superimposed during tensile testing may either decrease easy glide, when supporting the moments caused by gripping, or increase it, when cancelling the gripping moments.38 This interpretation of the authors&apos; results, emphasizing the special importance of secondary slip near the surface, is also consistent with the earlier results of Rosi.41 Copper crystals alloyed with silver in the surface layer show greatly increased easy glide compared with pure copper. In addition, the easy glide slope is reduced. The effect of bulk alloying in extending easy glide has been well established and has been interpreted as indicating the relative difficulty of secondary slip in alloy crystals. Since non-basal glide is difficult in zinc crystals, the effects of surface removal during deformation may be less important. Experiments to test this idea are in progress. I. R. Kramer and L. J. Demer (authors&apos; reply)—The authors wish to thank Dr. Alden and Dr. Fleischer for their discussion. Our interpretation of the data in the paper is that dislocation motion is obstructed by "debris" which starts to form at the surface and extends towards the interior of the crystal with further plastic deformation. The fact that we did not find a reversion from Stage II to Stage I by surface removal shows that in Stage II the "debris" fills the entire cross-section of the specimen. Drs. Alden and Fleischer take the view that bending stresses due to the grips are responsible for the

Jan 1, 1962

Air tabling of zircon-rich non-conductor products containing quartz enables most of the fine quartz present to be rejected without a markedloss of zircon. The coarser quartz in the air table feed can be separated from the zircon by screening one or more air table products, the oversize products containing most of the quartz and little of the zircon. Air tabling, with or without screening, is more efficient than wet tabling alone for the removal of fine quartz, but not for the removal of coarse quartz. Practically all of the quartz can be separated from the zircon by using wet tabling in conjunction with hydraulic classification, or by using air tabling in conjunction with dry launder treatment, in which a degree of sizing takes place that is advantageous for subsequent air tabling.INTRODUCTIONBack-dune and inland beach sand deposits usually contain fine wind-blown quartz, and neither spiral nor wet table concentration, alone or in conjunction, makes a clean separation of heavy minerals from quartz. Many rutile plants recover rutile and zircon from a low-quartz, wet-table concentrates by means of magnetic and electrostatic separation; some rutile and zircon are lost in the table tailings. Other rutile plants, and two of the ilmenite plants in Western Australia, recover rutile or ilmenite respectively, from a spiral concentrate containing several per cent of quartz, and then subject the non-conductor product to an additionalgravity concentration process to separate the zircon from the quartz. Some zircon is lost in the additional gravity process, but all of the rutile or ilmenite in the spiral concentrate is, or should be, recovered as high-grade concentrate. The higher recovery of rutile or ilmenite by this treatment method is offset by the expense of drying part of the feed twice, as a wet process is usually used to separate the quartz...

Jan 1, 1962

By D. L. Albright, R. W. Kraft

Solidification experiments were conducted with the objective of testing the theory of eutectic colony formation. Appropriate control of variables in tests on a series of high-purity aluminum-copper specimens of eutectic composition resulted in the observation of three types of eutectic microstructures, these being a unique structure consisting of lamellae essentially parallel to one another, a banded structure, and the colony structure. Lamellar faults, which are morphologically similar in many respects to edge dislocation models in crystals, produced a complex substructure in these specimens. SOLUTE rejection at the advancing solid-liquid interface of a unidirectionally solidified single-phase metal can cause the liquid immediately in front of the interface to become constitutionally super-cooled below the equilibrium liquidus temperature. Constitutional super-cooling occurs if the solidification rate, R, is too rapid, or if the thermal gradient in the liquid at the interface, G, is too low. 1 This constitutionally supercooled layer in turn stabilizes a cellular rather than a planar interface.&apos; A similar cellular interface has been observed when lamellar and other types of eutectics were unidirectionally solidified, and it has been shown that the cellular interface led to the formation of eutectic colonies.&apos; The lamellar structure is fan-shaped at the edges of colonies (which correspond to valleys or grooves in the cellular interface) because the lamellae grow normal to the local interface. One of the possible mechanisms which might cause the formation of the cellular interface, in the case of solidifying eutectic alloys, is constitutional supercooling of the liquid with respect to a third component rejected by both phases of the eutectic.3,4 On the basis of the analogy between the solidification of single-phase metals and binary eutectics, a eutectic alloy should solidify with a planar interface if the ratio of G/R is sufficiently high to compensate for any impurity which might be present and causing constitutional supercooling. The fan-like microstruc-ture of eutectic colonies should not occur under these conditions and the lamellae should be parallel to one another and to the solidification direction for extended distances. The experiments conducted in this investigation were designed to test these ideas. Following a resume of the experimental procedure, the various microstructures observed during the study are described, and their relationship to the growth conditions which produced them is discussed. EXPERIMENTAL PROCEDURE The eutectic between an aluminum solid solution and 0 phase (approximate composition CuA12) was chosen for this work for the following reasons: it was known that a lamellar structure forms, the eutectic temperature is low enough to facilitate experimental work, and the components can be procured commercially in a very pure form. High-purity copper (est. 99.999 pct Cu, obtained from National Research Corp.) and spectrographic aluminum rods, having impurities other than copper estimated to be Zn-15 ppm, Mg-10 ppm, Fe-3 ppm, Na-2 ppm, Cd-1 ppm, and Mn < 1 ppm, were melted in a stabilized zirconia crucible in a vacuum induction furnace at a pressure of 10 pof Hg. The melt was superheated to about 1000°C to assure mixing, cooled to 780°C and cast into an investment mold which yielded sixteen cylindrical specimen blanks 1/2 in. in diam and 5 1/2 in. long. The casting was allowed to solidify under vacuum. This master heat had an analysis of 32.6 wt pct Cu and 67.4 wt pct A1 by difference. The cylindrical specimen blanks were remelted and solidified unidirectionally in an apparatus illustrated schematically in Fig. 1. An RF induction coil heated

Jan 1, 1962