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By R. I. Jaffee, F. C. Holden, H. R. Ogden

The effects of grain size and shape on alloys of titanium with nitrogen and aluminum have been determined. Increasing a grain size decreases strength and hardness and increases impact resistance. Quenching from the ß field produces subgrain markings delineating a plates in Ti-N alloys but not in Ti-AI alloys. This suggests a precipitation from the high nitrogen alloys. ALPHA titanium alloys are single-phase alloys with the hexagonal-close-packed structure of a titanium. If these alloys are worked and annealed within the a field, equiaxed structures result in which strength is derived from the solid solution of the alloying elements present. Strain hardening can be used to increase further the strength of a titanium alloys. This is the only other mode of strengthening the a type of alloy. Quenching from the ß field has been noted by many investigators to have little effect on the strength of iodide titanium and on commercial titanium. Ti-A1 alloys were found to be little different in hardness, whether annealed in the a field or quenched from the ß field.' These facts illustrate a characteristic of a titanium alloys: they are insensitive to heat treatments from the ß field. Underlying this heat-treatment insensitivity are the facts that the a-ß field is generally narrow in a titanium alloys, the transformation-temperature range increases with a-stabilizing content, and the a solubilities of the alloying elements are greater than the ß solubilities. When quenching is done from the ß field, there is no supersaturation of the alloying elements in the acicular transformation structure produced. Welds in a titanium alloys generally are ductile, because no transformation hardening occurs during cooling.1,2 Other desirable features of a alloys are: no thermal-stability problem, excellent toughness, and retention of strength at elevated temperatures better than a-ß or ß alloys of comparable room-temperature strength. The prime factors governing the properties of a titanium alloys are the amount and kind of solute present. This can change the a phase from a soft, tough material into a hard, brittle material with no apparent change in microstructure. Moreover, brit-tleness can exist over a wider alloy-content range, without change of phase, than in most other metals. The solutes for a titanium may be divided into interstitial and substitutional types. Oxygen and nitrogen dissolve interstitially in rather large amounts, extending well through the brittle range, and the transformation-temverature ranges are raised in the process.:' , carbon has a maximum interstitial solubility of about 0.5 pct at the peritectoid temperature, while at lower temperatures the solubility decreases to about 0.2 pct.3,5 Substitutional a solutes include aluminum and tin. Aluminum has a high a solubility of 25 pct Al, and increases the transformation-temperature range markedly.6,7 Tin has a high a solubility of about 20 pct, but has a relatively innocuous effect on the transformation-temperature range.' The choice between interstitial and substitutional solutes generally has been conceded to the substitutional solutes because of a belief that they do not have as adverse an effect on ductility and notch toughness. However, a recent investigation8 on the effect of hydrogen on titanium has shown that this element, which is not under compositional control, has a powerful detrimental effect on notch toughness. Hydrogen was shown to form a hydride which is practically insoluble (about 0.002 pct) in a titanium at room temperature, although the solubility at the eutectoid temperature of about 300°C is relatively high, about 0.16 pct. Limited data were presented on the effect of hydrogen on a alloys, where the same impairment of toughness as in unalloyed titanium is found. The work reported here describes the effects of interstitial and substitutional solutes on 1—the mechanical properties of high purity titanium free of titanium hydride and 2—the influence of structural variables on these properties. Nitrogen was selected as an example of an interstitial solute with high solubility and aluminum as a substitutional solute with high solubility. All compositions were well within the ductile range, since it was not intended to study the brittleness problem here, but to study only the factors influencing optimum mechanical properties. Procedures The alloys were prepared from iodide titanium as 1/2 Ib ingots double melted to insure homogeneity.

Jan 1, 1955

By G. A. Moore

A brief review is given of methods designed to produce metallic iron of high purity, and typical results are listed. A recent method, utilized at the National Bureau of Standards, consists of the extraction of ferric chloride by ether, reduction of this ferric chloride to ferrous chloride, further purification of this chloride, and the subsequent electrolytic deposition of metallic iron. iron produced by this procedure apparently is softer than, and otherwise different in properties from, any iron previously prepared and contains appreciably smaller amounts of impurities. THE history of attempts to produce "pure" iron reaches to antiquity and it may be presumed that each ancient armorer who succeeded in making a better steel concluded, correctly, that he had done a better job of removing the "base metals," and incorrectly, that he now at last had a "pure" metal. Early metallurgical papers mentioned use of "pure iron" in making alloys—this "pure" iron in most cases being inferior to some commercial stocks of the present time. Improvement has been continuous, and usually at a sufficient rate to convince each succeeding group of workers that they, at last, were using the really pure metal (until the analysts also improved their techniques to again discover the impurities). These adventures were reviewed in some detail by Cleaves and Thompson.' Although the ores of a metal may be abundant, difficulties in extracting it may make the pure metal very rare. When impurities are restricted to a total of a few parts per million, nearly all pure metals become rarities. Lead, copper, gold, mercury, silver, zinc, aluminum, bismuth, and the six platinum metals are claimed to be available with total impurities ranging from 2 to 50 ppm. The present small and scattered world supply of so-called "pure" iron holds an unimpressive place in another group of 16 metals having approximately 100 ppm of foreign material. Of about 20 less rare metals, only the platinum metals are more costly to prepare. While the production of such rare varieties of iron may appear insignificant in the presence of thousand-ton operations with 95 to 99 pct metal, it must be emphasized that all researches on commercially interesting irons and steels are in fact studies of the modifications of the properties of iron by additional materials. Until the properties of high purity iron are directly measured, all ferrous research must operate without known base values. Traces of impurities may affect the properties of a metal in many ways. Infinitesimal traces of solutes, by disturbing the electronic configuration, greatly change the electrical properties of transistors and semiconductors2-3 and slightly larger traces might alter these quantities in iron. Soluble impurities which disturb the perfection of lattice arrangement not only may alter the magnetic constants and electric properties, but by their close association with dislocation phenomena probably control the very existence of the "yield point"; determine the value of yield stress; and perhaps control the selection of slip and cleavage planes. It has been speculated that impurities might even cause the allotropic transformation in iron, but in any case their rearrangement must contribute to the unreliability of heat capacity and other thermodynamic measurements. Impurities which do not remain in solution may cause even greater effects on the properties. Microscopically visible amounts of phases other than ferrite can be found in all high purity irons which have come to my attention. It can be calculated that from 50 to as little as 2 ppm of an insoluble material might be sufficient to completely film all grain boundaries in irons having grain sizes from ASTM Nos. 10 to 1. Should this occur, such films, even though invisible, may be very important in fracture problems, especially at extremes of temperature:' Studies of grain growth and diffusion normally imply consideration of a single-phase system, hence, in the presence of insoluble impurities they can be expected to give ambiguous data." High purity iron is also in demand for use as chemical and spectro-chemical standards; for work in classifying the lines of the iron spectrum; for biological work in nutrition; and for work in nuclear physics. where the presence of some sensitive

Jan 1, 1954

By B. R. Hollebone

The chemical action of molten anhydrous pyridinium chloride (pyridine hydrochloride) on oxy salts and ores of some Group IV and V metals are discussed-in particular zirconium, hafnium, niobium (columbium) , and tantalum. Laboratory-scale experiments are described whose results suggest that this reaction might provide a practicable means of converting ores of these metals to the anhydrous metal chlorides. Experimental results are given which provide some insight into the nature of the reactions and some of the compounds which could be present at intermediate stages. The treatment of ores of the more refractory metals is difficult and expensive and often demands the use of gaseous chlorine, hydrogen fluoride, or other reagents which are, if nothing else, expensive and dangerous to use. This situation is, of course, due to the strong metal-oxygen affinity resulting from the high charge and the small size of the metal ion which combine to produce such high lattice energy in the metal oxide as to defeat standard reduction methods. Thus, the characteristic of these metals which leads to one of their most important properties—corrosion resistance—is the main hurdle in obtaining the metal. Many common methods' for treating ores of zirconium and niobium (columbium), for example, proceed as directly as possible to the preparation of anhydrous halides. These halides are purified by now standard processes of solvent extraction, fractional distillation, and so on. This paper reports on preliminary stages in the development of a method of treating these ores—particularly of niobium—so as to prepare the anhydrous, volatile halides by the use of chemical reagents which are much more easily handled than those used at present. CHEMICAL PRINCIPLES The solvent action of aminium halides has been referred to periodically in the literature over several decades. The chemistry of pyridinium chloride has been discussed particularly by Audreith2 and Starke.3 However, since this is not familiar chemistry in its nonaqueous setting, it is perhaps well to point out some general metallurgical principles and applications. One can use, as point of departure, the fact that HC1 dissolved in pyridine is an acid very much the same as aqueous HC1. It thus gives essentially all the reactions of the HC1 with which we are familiar. However, when the ratio of HC1:pyridine reaches 1:l (a ratio far higher than is possible with H2O) the solution becomes solid C5F5NHC1, pyridinium chloride.* Inter- estingly, the acidic properties of HC1 persist in this medium, although they are manifest only in the molten state of the compound. Some typical reactions of divalent metal compounds which we have carried out in our laboratories are the following: 2PyHCl + Zn — (ZnCl2) + H2 + 2Py 2PyHCl + MnO — (MnCl2) + H2O + 2Py 2PyHCl + CuS — (CuCl2) + H2S + 2Py 2PyHCl + CaCO3 — (CaCl2) + H2O + CO2 + 2Py In these equations, the parentheses indicate a solvated compound which in water would be predominantly a hydra ted cation but which in molten PyHCl will more likely be a complex chloro-anion of the type MC14-. Some important physical properties of pyridinium chloride (PyHCl) are given in Table I. One sees from the data in Table I that at the temperature of molten pyridinium chloride both water and pyridine will boil away. Thus the system will be kept anhydrous. For this reason the reaction 2NbCl5 + 5H2O— Nb2O5 + 10HC1 has no counterpart in molten PyHCl. Instead, the chloride is made even more stable by the formation of a hexachloro complex: Nb2O5 + 12PyHC1 — 2PyHNbC16 + 5H2O + 10Py One interesting property of these complexes is their thermal instability which for the case of niobium can be illustrated as PyHNbCl6 — PyHCl + NbCl5 With a view to possible use of this chemistry in ore treatment, we have attempted to dissolve Pyrochlore (essentially FeO - Nb2O5) and recover the NbC15 from it.

Jan 1, 1968

By J. M. Blank, V. A. Russell

When the nucleation of silicon on a sapphire substrate is accomplished by gradually decreasing the substrate temperature while subjecting it to a constant impingement rate of hydrogen and silicon tetrachloride, the resulting deposit is characterized by widely separated islands of silicon scattered over an "open sea" of sapphire. Analysis shows that nucleation takes place mainly on sites of large adsorption energy, about 85 kcal per mole, and small surface concentration, about 108 cm-2. Crystal growth proceeds rapidly on these nuclei and results in enough depletion of Sicl4 from the ambient gas to suppress further nucleation. The technological importance of single-crystal films on dielectric substrates has prompted considerable work on the deposition of silicon on sapphire. This paper is concerned with the deposition of silicon, by the reduction of silicon tetrachloride with hydrogen, onto heated sapphire substrates. The apparatus consisted of a temperature-controlled container for the silicon tetrachloride along with gas lines and flow meters necessary to convey a hydrogen-silicon tetrachloride mixture to a reaction chamber constructed of quartz tubing. Heat for the substrate was provided by means of an inductively heated graphite susceptor. The observations pertinent to the present discussion were made with an American Optical Co. high-temperature microscope which allowed us to make motion pictures of the deposition process at a magnification of approximately 50 times. Two main categories of experiments were carried out: one on determination of critical condensation temperatures and the other on the deposition of epitaxial silicon films on the sapphire substrates. Critical condensation temperatures were determined in the traditional way by raising the substrate temperature well above that at which condensation could be expected at the impingement rates being studied and then gradually lowering the temperature until the condensation of the first silicon was observed. This was done initially with ellipsometry-type detection but it was soon discovered that the deposits were occurring as widely separated islands and groups of islands scattered over an "open sea" of sapphire. We have called these archipelago formations. They were most easily detected by optical microscopy. Data gathered from experiments of this type have been collected in Table I. Motion pictures of the formation of archipelago patterns show that the nucleation period lasts about 10 sec if the substrate temperature and impingement rate are kept constant. Essentially all of the nuclei are formed in a few seconds and all subsequent silicon deposition merely adds to the size of the established nuclei. After an archipelago formation has matured at a given substrate temperature and impingement rate, it is very difficult to stimulate any further nucleation in the open space between islands. Lowering the substrate temperature will occasionally stimulate nucleation but increasing the impingement rate hardly ever produces any more new nuclei. It should also be emphasized that the nucleation rates appear to be very small, about 104 cm-2 sec-1. They will receive special attention in the analysis section. Another series of experiments was performed employing a systematic variation of substrate temperatures and impingement rates approximating those expected to produce epitaxy. Sapphire substrates with surfaces normal to the 2233 direction were used. In contrast to the procedure that produces archipelago patterns, these films were deposited by raising the substrate temperature to a desired value at which time the silicon tetrachloride and hydrogen flow was begun. Of course, these depositions produced mainly films that were continuous. After removal from the deposition chamber, the substrate and silicon film were examined microscopically to determine the nature of the deposit and by X-ray diffraction to determine the extent to which a single-crystal film had been achieved. Results of these experiments are summarized in Table 11. Of interest for the present analysis is the fact that epitaxy appears to be confined to a fairly narrow temperature range between about 1050" and 1150°C. This also will be discussed in the analysis section. ANALYSIS In this section we shall apply nucleation theory to the data presented above with the objective of testing

Jan 1, 1967

Jan 1, 1926

By W. B. Hickman, J. J. Pickell, B. F. Swanson

Many physical properties of the porous media-immiscible liquid system are dependent upon the distribution of fluids within the pores; this in turn, is primarily a function of pore structure, liquid-liquiri interfacial tcnsion and liquid-solid wetting conditions. The cnpillary pressure hysteresis process provides a means of investigating the influence of pore structure upon fluid distribution for consistent sur/acc conditions. Invcstigntiot2s indicate that residual non-wetting-phase saturations /ollozuir,g the imbibition process (i.e.,wetting phase displacing nor2-wctting phase) are dependent upon both pore structure and initial non-raetting phase saturation and suggest that residual fluid is distributed as Discontinuous ,globules, one to a few pore sizes in dimension, thrnugh the entire range 01 pore sizes originally occupied. It clppears that air-mercury capillary pressure dala adequntely rellect the distribution of fluiris in a water-oil system when strong wetting condition preliczil. An oil-air counter-current imbibition technique has also been found to provide a rapid rneans of obtaining residual-initial saturation data. In a majority of cnses, rcsidual saturations detf-rniinecl from the oil-air or air-mercury process reasonably approximate residual oil saturation following water drive of a strongly water-wet medium. INTRODUCTION A reliable estimate of recoverable reserves depends not only on the amount of original oil-in-place but also on pore geometry and distribution of fluids within the pores. A critical parameter determining the recovery from a reservoir under waterflood, for example, is the amount and distribution of residual oil within the various rock types present. The purpose of this paper is to investigate the mechanism of capillary trapping and assess its importance in laboratory measureqents of residual oil saturation. The degree of wettability of a reservoir rock is recognized as an important factor in waterflood or imbibition experiments. In this paper, however, only the water-wet case has been considered. Considerable experimental evidence1 suggests that for water-wet rocks, capillary forces predominate in tile distribution of fluids and that viscous forces in the range normallv of interest in the reservoir have a minimum influence on residual oil saturation. It follows that if the ultimate recovery is controlled by pore geometry, a unique residual non-wetting phase saturation should exist for a given set of initial conditions. Two laboratory procedures.found to be extremely useful in the study of pore structure and degree of fluid interconnection at various saturations are decribed. Although air-nercury capillary injection curves have been used2 previously to characterize the drainage case, the withdrawal or imbibition case can provide valuable supplementary data. The air-mercury process, however, has several disadvantages; it is difficult to run in a sufficiently accurate manner, mercury does not always act as a strongly non-wetting liquid and in the air-mercury process the sample is rendered unsuitable for future analyses. An alternative process is described in which air is the non-wetting phase and naptha, hentane, octane or toluene is the wetting phase. INTERFACIAL TENSION AND CAPILLARY PRESSURE Interfacial tension between immiscible fluids is due to the difference in attraction of like molecules as compared with their attraction to molecules of the neighbouring fluid. This net attraction results in a tension at the interface. To extend the interface; thus, interfacial tension s can also be thought of as free surface energy. Interfacial tension is normally expressed as dynes/cm, and interfacial energy is measured in ergs/cm2 hence, both have dimensions ml A 2 and are numerically equal.

Jan 1, 1967

By J. P. Boisseau, C. N. J. Wagner, E. N. Aqua

An analysis ulas made of powder-paltern peaks from cold-rolled polycrystalline copper and from copper powders, compacted into briquets (1 in. diameter) with pressures up to about 106 psi. Powder-pattern peaks from both contact faces were measured with a diffractometer and CuKa radiation. Laltice-parameter measurements indicate the presence of residual stresses in the bulk specimen of the order of a - -10 kg per sq mm after 93 pct reduction in thickness, and give some evidence for the occurrence of deformation stacking faults (probability a - 0.003) in both bulk and powder samples. Fourier analyses of the line profiles were carried out on the (111) - (222) and (200) - (400) Pairs of reflections. The particle sizes decrease rapidly with increasing deformation and reach asymptotic values of De (111) = 550A and D, (200) = 350A at about 25 pct reduction in thickness or 80,000 psi pressure for compaction. The anisotropy of the particle sizes indicates the presence of microtwins and stacking faults on (111) planes. The rms strains increase also with deformation and reach limiting values of 2 x 10-3 in the [100] direction and 1 x 10-3 in the [Ill] direction at a distance L = 100A normal to the reflecting planes. THE diffraction of X-rays in cold-worked, polycrystalline, fcc metals and alloys yields Debye-Scherrer patterns in which the individual (hkl) lines may show a broadening, a shift, and an asymmetric shape.' These effects can be explained by the fragmentation of the small, coherently diffracting domains, the presence of residual elastic strains in the lattice, and the formation of stacking faults. X-ray studies of stacking faults in fcc metals and alloys have been methodically performed during the last few years, but so far most of the investigators dealt with cold-worked powder specimens obtained by filing.2-8,10-19 In such specimens, the crystals are randomly oriented and the average elastic strains are assumed to be zero, so that the observed peak shifts are due to stacking faults only. The agreement between X-ray diffraction theory1,20 and experiment is generally good. On the contrary, cold-worked, polycrystalline bulk specimens (after wire drawing, rolling, plastic deformation by tension or compression, etc.) contain residual elastic strains, which may not average to zero in the surface of the specimen and show very strong preferred orientation of certain lattice planes (texture) parallel to the specimen surface. Nonzero elastic strains also produce peak shifts, the magnitudes of which depend upon the crystallographic orientation of the reflecting lattice planes in elastically anisotropic materials as well as on the type of plastic deformation and which have to be taken into account when measuring stacking-fault probabilities in deformed bulk specimens.21-23 The purpose of the present investigations was to perform a detailed X-ray analysis on a bulk specimen of a fcc metal deformed by rolling at room temperature and on powder of the same material deformed by compaction, and to compare these results with those previously obtained on cold-worked filings.18 Pure copper was chosen for this study since it is known to produce only a small quantity of stacking faults by filing at room temperature.3,16,17,19 The residual elastic strain in the surface of the bulk copper should be the predominant factor determining

Jan 1, 1965

By G. J. W. Kor, F. D. Richardson

The sulfide capacities a1 1500°C of slags in the systern CaO + CaF, +Al2O3 have been measured by bringing samples into equilibrium with gas mixtures made from CO + CO2 + SO, + N2. The capacities are negligzble both JOY CaF, and CaF, + Al2O3 melts but when lime is present even at 20 wt pct capacilies as high as 30 x lom3 can be obtained. The results have yielded information concerning the liquidus at 1500°C and fluoride-oxide melts in general. The slags used in electroslag refining contain substantial amounts of calcium fluoride. Robinson and Grainger' report that good results can be obtained by using slags of the approximate composition 70 wt pct CaF2 + 30 pct Al2O3. It has also been reported2 that a mixture of 50 pct CaF2 + 30 pct A12O3 + 20 pct CaO makes a good slag for general use. In view of the fact that very low sulfur contents are claimed for ingots produced by the electroslag process. studies have been made of the sulfide capacities [c, = wt pct S (PO2/Ps2)1/2 at 1500°C. of slags consisting of pure calcium fluoride, and of its mixtures with lime and/or alumina. These studies have also provided information on the phase diagrams. The slags were brought into equilibrium with gas mixtures prepared from NZ + CO + CO2 + SO2. Because CaFz is volatile and also easily hydrolyzed. measurements were made of its loss in weight in various flowing gas mixtures. EXPERIMENTAL Procedure. The apparatus and procedure were the same as described previously. Both platinum and iridium crucibles were used (height and inner diameter about 1 cm), but those made from iridium were stronger and able to withstand a greater number of experiments. In each experiment two crucibles were set in an alumina support and 1 g of slag mixture was divided between them. The materials from each crucible were analyzed separately after being brought to equilibrium with the gas, and then quenched in the water-cooled end of the reaction tube. Materials. Alumina and lime were prepared as de-scribed previously.4 Calcium fluoride was obtained by igniting Analar calcium fluoride in a platinum boat at about 800°C in a stream of pure dry nitrogen: the product was cooled in a desiccator. The slags were produced from mixtures of the powdered constituents, these being melted together in the course of each equilibrium experiment. The sulfur analyses and the X-ray diffraction meas- urements on the solidified slags were made as described previously.4 From the latter it appears that the CaF2 contained less than 0.5 mol pct CaO. RESULTS Values of (ps2/po2) for the Gas Mixtures. The re-sults have been represented in terms of (ps, /Po,)"? for the various gas mixtures used. The va1;es of this function at 1500°C are listed in Table I: they were calculated from the data cited previously for calculations at 1350°C 4 Weight Losses with CaF, and CaF, + CaO. The re-sults of the weight loss measurements* at 1500°C for

Jan 1, 1970

By R. G. Gifkins

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

Jan 1, 1960

By J M. F Clout

The low-grade clay-rich -1.0 mm fraction of fine iron ores have often proved difficult to upgrade and capital intensive to process when using traditional wet beneficiation technology including single or two stage hydrocyclone desliming, wet high intensity magnetic separation (WHIMS), spirals and final dewatering using fine screens. Very fine (<0.010 mm) clay-rich slimes simply follow the water split to the hydrocyclone underflow where it often impedes the subsequent processing performance of any downstream spirals and can result in troublesome direct dewatering of hydrocyclone underflow. The -1.0 mm fraction in goethitic iron ores is typically considered as waste. A new two-stage wet gravity separation flow sheet, referred to as the ædesandÆ process, has been designed to overcome these issues for the upgrading of low-grade clay-rich goethitic or hematite-quartz fine iron ores. The desand process is designed to treat the -1.0 mm range from -8.0 mm natural fines, to recover a -1.0 +0.038 mm higher-grade fraction by rejecting to tailings any low-grade clay-rich ultrafines and low density sand-size fine chert/quartz gangue and shale.The desand process consists of wet screens with a nominal 0.7-1.0 mm cut point which direct the undersize to hydrocyclones. The hydrocyclone underflow is then fed to upcurrent classifiers where the classifier middlings is sent to spirals and classifier and spirals concentrates are then dewatered using vacuum belt filters or fine screens. The three product upcurrent classifier is employed to further deslime the hydrocyclone underflow, producing firstly a coarse final concentrate, and then a deslimed middlings for feeding to spirals as well as a 0.100 mm clay and fine quartz or banded iron formation (BIF) sand in final overflow for feeding to the residue thickener. The upcurrent classifier middlings provides the spirals with a significantly cleaner feed material than traditional methods, with the end result that the spirals do not silt up with slimes and therefore can continue to run at their optimum. The upcurrent classifier and spirals form a complimentary pair, with the upcurrent classifier better able to send coarser, acceptable grade particles to concentrate and fine slimes to tailings whilst allowing the spiral to better reject coarser, subgrade low specific gravity particles. Test results for the Mayoko-Moussondji iron project, Republic of Congo, using upcurrent classifier-Wilfley Table (simulating spirals) gave acceptable mass recovery from run-of-mine (ROM) and Fe recovery from hydrocyclone underflow for HEMCOL (6.2 per cent mass recovery from ROM/43.1 per cent Fe recovery) and HEMBIF2 (5.1 per cent mass recovery from ROM/22.3 per cent Fe recovery) mineralisation types. The desand process also enables improved dewatering of -1.0 +0.038 mm product from a clay-rich plant feed.A number of new wet plants in the Pilbara use the desand flow sheet including FMGÆs Cloudbreak and their two Christmas Creek plants. Many potential new applications are being explored, with new iron ore plants in India as well as those being proposed for West Africa. Operational experience has highlighted the importance of providing clean process water to the upcurrent classifiers as well as ongoing design improvements including increased wear life, reduced maintenance and enabling a more steady feed rate to spirals.CITATION:Clout, J M F, 2013. Beneficiation of fine iron ores using the desand process, in Proceedings Iron Ore 2013 , pp 337-348 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Aug 12, 2013

By J. E. 214-000-000-010 Warren, M. R. J. Wyllie, T. Meidav, L. Scharon, R. Uhley, A. J. deWitte

By considering the stoichiometry of the underground combustion process, an equrztion was derived relating the point velocity of the combustion front as a function of the air flux, fuel content, efficiency' of oxygen uitilization, hydrogen:carbon ratio, and ratio of carbon dioxide In carbon monoxide produced. In addition, an equation for cnlcrllating the amount of injected air necessary 10 produce the oil from I Cu. ft of reservoir space was derived. This equation has a direct bearing on evaluating compression costs for the process. Values calculated from these equations are in good agreement with experimentnlly obscrvcd values obtained from laborator) tube runs reported in the literature. The equations are also u\eful for atlcrlyzinf: experinlental data for inconsistencie.r.. I NTRODUCTION The injection of energy in the form of heat into an oil-bearing formation as a means of increasing the recovery of oil has been the subject of much discussion and experimentation as far back as 1920. The ideas have ranged from the injection of steam to the direct use of electricity as a means of getting thermal energy into a formation. However, most laboratory and field studies have been confined to the process whereby a portion of the crude in the reservoir is burned to generate the necessary heat to increase the mobility of the oil by reducing its viscosity. A recent paper by W. L. Martin, et al.', described the results of a number of laboratory experiments in which the combustion process was studied in a sandpack. Studies such as this indicate that with the temperatures involved, the oil is partially coked in this process and it is this coke which provides the fuel for combustion. The combustion of this residual coke can be analyzed theoretically by applying simple stoich-iometric principles to the combustion process. It is the purpose of this paper to compare the results reported in these experiments with those obtained from theoretical considerations. The variables studied by Martin, et al, among others, include combustion front velocity, air flux, oxygen utilization, fuel concentration, ratio of carbon dioxide and carbon monoxide in combustion gases, and the hydrogen:carbon ratio of the residual fuel. All these variables come into consideration when the stoichiometry of the combustion process is studied. The experimental conditions and results are tabulated in Tables 3 and 4 of Ref. 1. For purposes of comparison with calculated results, it was necessary to change the units of a number of the variables. UNDERGROUND COMBUSTION STOICHIOMETRY The combustion or oxidation of the carbonaceous residue or "coke" on the sand can be described in terms of the equation: where n is atomic ratio of hydrogen to carbon, m is ratio of moles of CO2 to CO produced, and CH. is taken as the unit molecular weight, realizing that actually the coke has a large range of high molecular weights. Assuming that all the fuel laid down in the sand is burned, the ratio of moles of oxygen consumed to moles of coke can be written as follows. Moles 0MolesMolescoke In terms of moles O2 per pound of coke, where 12 + n is the molecular weight in pounds per mole. If the 0, consumed is measured in standard cubic feet (60°F and 1 atm) and the coke in pounds per cubic foot of formation, 2, then:

By M. A. Torcaso, P. Raimondi

To study mass transport in systems simulating oil recovery processes, different porous media were saturated with a mobile (carrier phase) and a stationary phase. Slugs of carrier phase containing a small amount of solute were displaced with pure carrier phase. By analogy to the chromato-graphic processes, the velocity of the solute can be predicted from a knowledge of the partition coefficient and the saturation provided that equilibrium between the two phases exists. Equilibrium was found to exist for different porous media, solutes and rates. The conditions were varied over the range normally encountered in the laboratory and in the field. The longitudinal dispersion of a solute undergoing interphase mass transfer was also investigated. INTRODUCTION The production of hydrocarbons by gas cycling, enriched gas drive and C02 or alcohol displacement involves, among other factors, relative motion between two phases and compounds, hereafter called solute, which are soluble in both phases. The solute is carried forward by the faster flowing phase at a lower velocity than the average velocity of that phase. Retardation of the solute is caused by chromatographic absorption and desorption in the slower flowing phase and by the degree of departure from equilibrium. At equilibrium the concentration of solute in the two phases can be related by the equation* CSw = K Cso ,............(1) where C, and C are the concentration of solute in the aqueous and oleic phases respectively and K is the equilibrium ratio, or partition coefficient. Displacement theories must contain an explicit assumption with regard to equilibrium, i.e., whether the compositions can be related by Eq. 1. The existance of equilibrium depends, in general, on the relative velocity between the phases. Unfortunately, other factors such as gravity segregation and viscous fingering, also depend on velocity. For this reason, whenever effects of rate on displacement were observed,2-4 it was practically impossible to discern what caused them — lack of equilibrium or the factors mentioned above. Equilibrium between phases has been the subject of extensive studies in fields such as extraction or chroma to graphy. It has received only small attention in flow through the type of porous media encountered in oil production.5 For this reason a method was developed which makes it possible to study the movement of a solute as it is affected by rate, type of porous media, partition coefficient and carrier phase, but in the absence of segregation or fingering. The information obtained enables one to determine when the assumption of equilibrium can be made. Briefly, the method consists of (1) saturating the core with a mobile and an immobile phase, (2) injecting a slug made up of the same fluid as the mobile phase and a small concentration of mutually soluble solute, (3) measuring the lag and the peak height of the slug at arrival and (4) correlating these variables with fluid properties such as partition coefficient and mixing constants of the medium. PROPOSED MECHANISM The principles of chromatography are combined with the equation of longitudinal mixing to predict the velocity of a solute slug compared to the bulk velocity and the peak height of a slug.6-9 The equation so obtained is valid under equilibrium conditions only. Therefore, a comparison between experimental and predicted results will give a measure of departure from equilibrium. This work was done with either the oleic or the aqueous phase being immobile. For simplicity, the following development is based on the case where the oleic phase is immobile. However, the treatment is the same in either case.

Jan 1, 1966

By Dwight K. Smith, Greg Carter

Studies have been conducted on The properties of many deep well cementing compositions to determine their Strength behavior over curing periods to 180 days at elevated tem-peratures and 3,000 psi pressure. This pressure results in essentially the .vat, compressive strength as that obtained with much higher pressures in ac-cordance with the findings of an API subcommittee ' These different compositions include API C1asses A, E, and F cements containig additives such as retarders, berrtorlite, heavy weight materials and pozzolans. All compositions except mixtures of Poz-zolrrrts and hydrated lime show from mild to severe degrees of strength lass over a temperature rang from -730 to 320" F after setting. Pozzolatl-time compositions actually gain in strength with time at these high temperatures. Other chemical find physical properties evaluated to observe their inter-relation.ship with Strength loss show very little correlation except in per-meability. As retrogression in strength increases, the permeability of set cement increases. X-ray difraction patterns on the set products indicate the formation of certain compounds having little or no strength value in those cementing compositions where strength loss was more severe. INTRODUCTION As a result of the growing trend toward deep well completions, a study has been made on the properties of the various cementing slurries presently in use at elevated temperatures and pressure. The strength of these compositions is of prime importance in selecting the most suitable material for use at high temperatures, to determine WOC time and the proper time to perforate with a minimum of shattering. Of primary interest in this investigation was the strength behavior of various compositions currently in use, and the effect of additives on cement after long periods of curing under severe conditions. Earlier investigators have pointed out that the strength of some cements will increase with increasing curing temperature to about 220 to 340" F, but at higher temperatures a loss in strength occurs at extended time intervals. Studies by the API Mid-Continent District Study Committee on Oil Well Cements' outlined a testing procedure whereby field conditions of temperature and pressure could be simulated in the laboratory.' It was observed that retarded cements undergo changes at elevated temperatures and some lose as much as 50 per cent of their early strength when cured at high temperatures. The scope of these tests was limited to curing periods of 1 to 28 days; additives were not covered in this study. Saunders and Walker' found that the use of additives influenced the strength behavior of cements at high temperatures, but studies were conducted only to a seven-day curing period. Ludwig and Pence' conducted an investigation of two types of cements under elevated pressures and temperatures in an effort to explain the causes of this loss in strength phenomenon. It was observed that with retrogression in strength there were other physical and chemical changes which took place as the cement aged. Today there are a number of cementing compositions available for use at well depths below 10,000 ft. Since all these earlier investigations were limited in curing time as well as the number and type of compositions studied, it was believed that a more extensive study should be conducted on the properties of cements at elevated temperatures, and this work should include those compositions actually in general field use at this time.

By N. J. Grant, H. Brunner

This paber is concerned with the determination of equations relating elongation to the amount of shear taking place both along grain boundaries and in slip planes of poly crystalline aggregates during creep. Certain discrepancies with previously used equations are pointed out. Grain boundaries were observed to become serrated during creep, but it is shown that this does not necessarily prevent further grain boundary sliding. Direct obser-vations of subgrain boundary ingration lead to the conclusion that this migration facilitates sliding along serrated grain boundaries. It is bointed out that the state of stress at triple boints is still unknown. MOST of the mechanisms of deformation contributing to elongation are shear processes, such as slip, kinking, grain boundary sliding, and twinning. For quantitative investigations of individual deformation mechanism it is necessary to know the equation which permits the calculation of speci-tnen elongation from measured amounts of shear. This calculated elongation must then be compared with the observed total elongation. The authors' special interest concerned grain boundary sliding during creep. Although this subject has already been investigated quantitatively by McLean,' Rachinger,' and Fazan, Sherby, and Dorn, calculations indicated that none of the equations used thus far to relate shear with elongation were sufficiently well founded. A basic study of this relationship was thus made and the results of this study (which do not entirely agree with those previously used) are presented. Most of the ideas set forth apply not only to grain boundary sliding but to other mechanisms of shear as well. THE SPEAR-ELONGATION RELATIONSHIP Basic Models—The relationship between shear and elongation is trivial in the simplest case of shear, which is shown in Fig. l(a). The vector A; designates the displacement across the shear interface, and Au, and Aut are its components parallel and normal to the tensile direction, respectively. It is evident that the specimen elongation due to shear is equal to the longitudinal component of the shear vector, and it should be noted that the normal component does not contribute to the elongation of the specimen (there are, of course, two normal components in a three-dimensional model). The model shown in Fig. l(b) may be applied to mechanical twinning and to subgrain boundary tnigration. In this case the width (h) of an already existing shear band increases by the migration of an interface, but the shear angle y (angle of mis-orientation in the case of a subgrain boundary) remains constant. The geometrical relationships indicated in Fig. l(b) permit this case to be reduced to the one shown in Fig. l(a). For the resulting elongation A6 we find: where AV/V = fraction of the volume of the specimen swept by migrating interfaces , and 1 = length of specimen. Thus, assuming for example that the angle of mis-orientation is 1 deg, and that P = 45 deg, we find that the specimen elongates 0.87 pct of its length if the entire volume of the specimen is swept once by such a subgrain boundary. An example of deformation by migration of subgrain boundaries is shown in Fig. 2. The specimen shown was repolished after 9.8 pct creep strain and the test then continued for another \ pct. Since the shear vector has, in general, a component normal to the surface, subgrain boundary migration results in the formation of an inclined band delineating the region swept by the subgrain boundary. These inclined bands become clearly visible when observed with oblique illumina-

Jan 1, 1960

By Wm. Moorhead

Safety Measures Employed at the Dawson Mines Preventive measures for eliminating and localizing explosions is a subject of special interest to Coal Mining operators at the present time. I shall endeavor in this paper to present the practical methods which have been developed at the mines of the Stag Canon Branch of the Phelps-Dodge Corporation, Dawson, New Mexico. Adobe Dusting Adobe is used for practically all dusting on the main haulage roads. It is obtainable in sufficient quantities adjacent to the mines. Loaded into railroad cars by a clam-shell loading crane, and transferred to the mine pit cars at the nearest available point, it is readily distributed along the motor roads by means of the mine locomotives. Of first consideration for adobe dusting is the preparation of the roadway. It is essential that all loose coal and dust be removed, at least to a depth of three or four inches below the top of the rails. The adobe, in a more or less moist condition is unloaded by hand from the pit cars and stored along the previously prepared roadway, to be later scattered to a depth of several inches over the floor, and over the ribs and roof such as is possible by the use of a shovel. The adobe soon loses its moisture and becomes pulverized. Due to the disturbance caused by passing motor trips, men and animals, the dust is effectively scattered along the ribs and roof of the roads. The velocity of the intake air aids materially in sustaining the suspension of this inert matter. Another scheme for distributing the fine dust in use is to chain the top of a pine tree to the rear of the trips, both empty and loaded. Dragging it along the motor roads stirs up the dust and aided by the intake air it is carried for long distances into the workings. The adobe is continually loosened and raked, all rock, coal, etc., being collected in piles and later loaded out in pit cars. One man is employed for each six thousand feet of entry. Dusting Main Return Air-Courses The air-courses are first thoroughly cleaned. All the loose coal and rock is loaded out, the ribs and roof washed down several times. Every five or six hundred feet, the stoppings between the main and return entries are broken through and small doors installed. Blowers are used to force the fine dust into the return air-courses through these openings. Thus suspended the dust travels a considerable distance before it is deposited on the floor, ribs and roof. The material used is chiefly adobe, sun dried, and screened on the outside. A two ton car load of this dust will cover several hundred feet of airway as very little loss occurs, often depositing from 2 to 6 pounds per running foot of entry. Methods of Insertion Blowers are used to force the dust into the main returns. One unit consists of a small Buffalo blower mounted on a truck with a two H. P. motor. A six-inch pipe is attached to the blower and runs the full length of the truck with a projection over the end. A hopper is built over the pipe and connected. Stove pipe or canvas tubing is led from the pipe through door in stopping. When the blower is started dust is fed into the

Jan 1, 1924

By S. J. Burns, W. W. Webb

The dislocation arrangements formed during unsteady propagation of cleavage fractures on (010) planes in LiF have been investigated by high-resolution etch-pit techniques and by X-ray diffraction topogvaphy. In impurity-hardened crystals, cracks propagating in any direction on (010) planes at velocities of about 103 cm per sec are usually accompanied by light plastic deformation which is enhanced wherever the crack is allowed to hesitate. Dislocations with [011] type Burger's vectors are often formed looped around the crack tip. They are dragged along with the crack tips leaving edge dislocations lying nearly parallel with the clearage surface about 5µ from it. These dislocations are easily overlooked since they may initially intersect with the cleavage surface infrequently and later may disappear from the crystals due to image forces during aging at room temperature. Although the plastic work associated with these dislocations is only comparable with the reversible (010) surface energy, an instability in crack propagation appears due to a limit of the velocity with which dislocations can be dragged along with the crack. Transition to a fully brittle nonplastic fracture mode occurs when the crack velocity exceeds the velocity with which dislocations can be moved by the stress field of the crack. TRANSITIONS between brittle and ductile modes of fracture appear to be common processes in the behavior of materials in which the flow stress is close to the stress at which brittle cracks can propagate. High-strength engineering alloys fit into this category and the transition from ductile to brittle modes of crack propagation may be associated with catastrophic failures in these important materials. The methods of theoretical mechanics indicate the geometrical conditions in which these processes may occur but the detailed mechanisms controlling the generation of dislocations in the initiation of the plastic mode and the process by which the loss of plasticity occurs on transition to the brittle mode are not yet clear. Since these mechanisms are not amenable to direct observation in engineering alloys we have chosen a semi-ductile alkali halide LiF as a model system in which to observe transition mechanisms between plastic and brittle modes of crack propagation. Cleavage cracks in this system are known to undergo a plastic-elastic transition at velocities between 103 to 104 cm per secl and dislocation configurations in LiF are amenable to study by optical-microscopic observation of dislocation etch pits2 and by X-ray diffraction topography.3 We have been able to identify a dislocation mechanism responsible for the transition from brittle to slightly plastic modes of crack propagation in LiF. A model based on this mechanism permits calculation of the critical crack-propagation velocity for this transition and indicates the importance of the stress dependence of dislocation velocity in determining the critical crack velocity. Of course, this model cannot be carried directly over to more complex materials but it is quite possible that its qualitative features are generally applicable. Dislocations intersecting fresh cleavage surfaces in LiF were reported by Gilman,4 by Forty,5 and by Wash-burn et a1.6 Such dislocations were construed to have been nucleated where the cleavage crack hesitated or stopped, near stress concentrators, such as cleavage steps, on the crystal face. The loci of such dislocations deposited On the cleavage plane in bands were called "stop lines" or "deformation zones". Gilman, Knudsen, and walshl measured the velocity of cleavage cracks in lithium fluoride by evaporating thin resistive strips on the crystal side and recording

Jan 1, 1967

By John W. Cahn

Tile avevage value of the mean curvature of surfaces in a specimen can be precisely delermined by sitrlple measurements performed on random sections or on 1 vojectiotzs of these surfaces. For surjaces enclosing particles, the quanlity is sllown to be velated to the probable tlurrrhev ot particles intevcepted by a random platne and, under certain conditions, to the perimeter of their Projected image and to the increuse in surjace area when the particles grow. Many of the velalionsl~ips are valid for any shape or size of the particles. THE recent growth of the field of stereology or quantitative microscopy is largely the result of the discovery of a limited number of rigorously defined geometrical parameters that can be precisely measured on random sections or projections of a structure without assumption about particle shape.' Such parameters have been the volume fraction and surface area and line length in a unit volume. The present paper introduces the average of the mean curvature of surfaces in a volume, and shows that it can be rigorously measured by counting methods alone. AVERAGE CURVATURE ON A PLANE Consider a curve y = v (x) on the xy plane. The curvature Kp in the plane at any point is given by Kp = (dZy/dx2)/[1 + (dy/dx)2]3/2. The average curvature along the curve may be defined as Kp = (1/L) fKpdl |1] where dl = [(dx)' + {dy)2]1/2 is the length of an element of the curve and .(dl = L is the total length of the curve. The integral on the right-hand side of Eq. [l] will be called the total curvature, It is dimensionless and readily evaluated by substituting d = arctan (dy/dx) to give ah which is the change in direction of the tangents to the ends of the curve, Fig. 1. Hence, Kp = (1/L)(?h) [2] It can also be seen that Eq. [2] is applicable in the limit of sharp corners. Even though the curvature is infinite at a corner, f Kpdl remains integrable and equal to the change of angle. The signs of the quantities Kp and dl are arbitrary and, if the areas adjoining the curve are equivalent, there seems to be no compelling reason to fix the signs. For a closed curve, however, it becomes worthwhile to use the signs to distinguish among different types of areas or phases enclosed. For such a closed curve AO = t2r and As a convention, we shall take the direction of the integration along the curve in such a way that the area or phase under consideration (henceforth called a) is kept to the left side of the curve, Fig. 1. Then Kp is positive where the curve is concave and negative where the curve is convex. For a closed curve Ad - +2n if the curve encloses a, and Ad = —2n if the curve is surrounded by a. PLANAR SECTIONS OF THREE-DIMENSIONAL STRUCTURE OF ISOLATED a PARTICLES Consider next a planar section of a microstructure containing particles of a in a matrix. We place no restriction on shape of connectedness of these particles, and begin by considering the curvature of only the boundary between a particles and matrix' Clumps of contiguous a particles are then treated as a single a particle. The two-dimensional section will show in a unit area na simple closed curves enclosing a particles and nh closed curves of holes, in-

Jan 1, 1968

By J. J. Arps

n approach to the study of the electrical properlies of drilling muds, their cakes and their filtrates was made by treating the drilling fluid as a porous medium. Lluring this study it was found that the weight pararneter was omitted from previous investigations on electrical properties. Patnode in 1949 made a similar approach to ,his investigation. His work showed that there was a variation of resistivity relationships with per cent Puid present in a given suspension. This present study ex-tends Patnode's investigation to one in terms of the solids fraction of the drilling fluids. Previous investigations were made on low weight muds where the effect of the rolids fraction was obscured. The following equationr were fitted to data taken from 94 field muds and 47 laboratory muds (see Tables I and 2). The parameter, C, is a complex function of the solidr content, or mud weight, of a drilling fluid. It was also found that for all drilling muds examined. A nomograph is presented combining Eqs. I and 2. INTRODUCTION It is generally recognized that the materials present in drilling muds affect the relationship between mud filtrate and mud resistivities. However, most electric log interpretations proceed with the assumption that the mud resistivity and temperature are the only important parameters needed to obtain a filtrate resistivity or a mud cake resistivity. Lamont1 suggests that only average relationships exist between mud cake, mud filtrate and mud resistivities. He indicates that there is limited accuracy when these intercorrelated factors are used since no other measure-able variable is apparent. A previous paper by Patnode indicates that drilling fluids may be considered to be a system of fluids in solid particles which may be correlated electrically in a manner similar to rock solids. 1 he equation for the resistivity factor. F = (per cent fluid) is satisfied for a given clay type in water, but the value of m varies as different materials are used in the water. The resistivity factor is not constant for a given amount of clay. As is suspected it varies as the solids fraction conducts electrical current. Since both weighting material and clay solids are present in commonly used drilling fluids, it is expected that both materials contribute to the variation of the m factor in Eq. 3. An extension of Patnode's work is presented in this paper to show some of the interrelations which exist between the resistivities of mud cake, mud filtrate and mud. Use of these data enable a more accurate calculation of mud filtrate and mud cake resistivities if only the mud resistivity and weight are measured. EXPERIMENTAL The measurements of mud weight, fluid and solids resistivity, alkalinity, and chloride content of mud samples were made in this research. Mud samples representing drilling fluids from 94 Louisiana and Texas wells (Table 1) and 47 laboratory-constructed systems (Table 2) were used in the experimentation. The measurements of the mud properties were made both in the field and in the laboratory. The tests on the properties of weight, alkalinity and chloride ion were standard tests as described by API specifications. The resistivity measuring devices were constructed in the laboratory for this study. For details on the resistivity equipment see Fig. 1. The fluid cell

At 5:30 p.m. a social hour was held for all RMCMI registrants on the lawn area south of the Gondola Lift House. This was followed by a western steak fry and dancing to the country western band, "The Cat's Night Out". MORNING SESSION Tuesday, June 29,1982 RMCMI golfers came out in force for a shot-gun start of the Championship Golf Tournament at Vail Municipal Golf Course which began its first session at 7:30 a.m. followed by a second at 1:15 p.m. The tournament was headed by William Carpender, chairman and his committee members Gary Bennewitz, Jr. and Gene Christmann. RMCMI members were treated to early morning rolls and coffee in the Conference Center preceding a showing of the RMCMI slide/tape program on enhancing the image of coal mining, by telling the story of the Institute. Following this, the meeting was called to order by President McKeever at 8:30 a.m. when he introduced Mr. Carl Terzian who presented a workshop entitled "Sure You Have an Image - But What Kind?". MR. McKEEVER: Good morning Carl. I see you're ready to address this bright and busy tail audience. One of the things that I really want to point out this morning and I knew we would have a second chance with Carl Terzian but Carl is someone that will leave a good lasting impression on you and what he will hopefully be talking about, as I remember, is that what he's saying here can be used personally, or for company, or for the Institute, or anything else on image. Carl is Chairman of the Board of Carl Terzian Associates. He is a prominent author, lecturer and consultant. He is headquartered in Los Angeles and he's nationally known: governmental affairs, man¬agerial development and executive speech training and has served nearly four hundred clients since 1969. Each year he travels nearly 300,000 miles to address conventions, conferences and sales and management meetings as a motivational speaker. Carl has been speaking professionally for more than twenty-five years. He was graduate magna cum laude 1957 from the University of Southern California where he was elected Phi Beta Kappa and student body president. He later served as State Department goodwill ambassador for President Eisenhower; public relations director for Lutheran Hospital Society of Southern California; dean and professor of political science and speech at Woodbury University and public affairs director for architect Charles Luckman. He has been honored for his civic and philanthropic and professional accomplishments by the Congress and State Department, California Assembly and Senate, City and County of Los Angeles, Her Majesty the Queen of England, and six times by the Freedom Foundation of Valley Forge. Carl, welcome to our Coal Mining Institute and it's been kind of a historical situation on Tuesday morning that we will probably have people straggling in after that wonderful steak fry that we had last night. You're very welcome to come and takeover the command. MR. TERZIAN: Thank you very much Ira. This gives me an opportunity for those who were in my luncheon audience yesterday to again thank you for giving me the opportunity of that platform and for the very kind comments that were made following the address. Those of us who had been working for some months with Ira, Charlie, Betsy and many

Jan 1, 1982

By R. G. Davies, R. H. Richman

Several techniques, X-ray diffraction, transmission electron microscopy, conventional, metallography, and mechanical property measurements are combined to investigate decomposition in the suPersaturated solid solution Fe-27 at. pct Be. The following sequence of structures for aging temperatures below 400°C is established: massive short-range order, pseudo-FeBe (L2o) order, Fe3Be (DU3) order, sinusoidal modulation of composition, general or continuous precipitation, and discontinuous or cellular precipitation. In addition to this sequence itself, several features of the individual stages are noteworthy; for example, when coherent modulations occur, their development is parallel to (100) everywhere in the specimen apparently without incubation, and both the wavelength and the composition amplitude of the modulations increase with aging time. Two types of discontinuous reaction are observed, depending upon the aging temperature. At low temperatures (<550°C) the boundary-nucleated variety of discontinuous precipitate predominates; but at higher temperatures (>600°C) the crystallographic variety occurs instead. Hardness and flow-stress measurements clearly reflect the quoted structure sequence. Some qualitative aspects of the structure changes and of the relationship between mechanical properties and structure are discussed. BERYLLIUM in solid solution markedly strengthens iron.&apos;" A recent study demonstrated that not only were supersaturated single crystals of Fe-27 at. pct Be very strong, but they deformed primarily by mechanical twinning.3 Such behavior, coupled with the decrease in solid solubility of beryllium in a Fe from about 33 at. pct at 1165°C to about 10 at. pct at 500°C4 as shown in Fig. 1, leads naturally to questions about property changes with aging in this system. In 1929 roll,1 and later Seljesater and Rogers,5 reported that useful increases in strength could be obtained by aging quenched Fe-Be alloys, but it was not until quite recently that any of the details of precipitation in these alloys were studied. Richman6 observed that both an Fe3Be superlattice (with a DO3 crystal structure the same as Fe3A1, illustrated in Fig. 2) and a modulated structure preceded the appearance of a discrete second phase in the 20 at. pct Be composition. Here, a modulated structure refers to a periodic composition fluctuation within one crystal, while its lattice remains coherent. Subsequent work on a Fe-Be alloys by Heubner7 and von Heimendahl and Heubner8 confirmed the existence of the modulated structure, although only an FeBe (L20) ordered structure was detected (also shown in Fig. 2). Both Rich-man and Heubner corroborated the large increases in hardness during aging reported earlier, but other mechanical properties were not examined. Since modulated systems are encountered relatively infrequently, the influence of coherent modulation upon mechanical properties is not well-known. With the accumulation of information about age-hardening systems, it has become clear that many precipitation reactions cannot always be described by the concept of heterogeneous nucleation at some lattice discontinuity followed by diffusional growth. Rather, complex sequences involving prior "preparation" of the matrix are quite common; that is, a transition structure occurs in the parent phase, instead of in some "nucleus" form. Delineation of such subtle sequences appears to be a worthwhile step toward the understanding of solid-state precipitation. Since not many structural progressions of comparable nature have been reported, the objectives of the present survey are to identify and elucidate the various

Jan 1, 1967