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By E. J. Rapperport, M. F. Smith

A presentation of the W-Ru constitution diagram is given. Techniques utilized in the determination of phase boundary values include electron micro-probe analysis of two-phased alloys and diffusion couples, as well as normal metallographic and X-ray methods. The primary features of the diagram are: 1) a terminal solid solution of ruthenium in tungsten with a maximum solubility of 23 at. pct Ru at 2300°C; 2) a terminal solid solution of tungsten in ruthenium with a maximum solubility of 48 at. pct W at 2205°C; 3) a o phase of maximum breadth about 6 at. pct based on the composition W3Ru2 which forms peritectically from the melt at 2300°C, and which decomposes eutectoidally at 1667 °C to form a twigs ten and 0 ruthenium; 4) a eutectic at 45 at. pct Ru and 2205°C with the products being o plus ß ruthenium. THE W-Ru diagram has previously been studied only in a cursory fashion. Raub and alter' obtained a 1400°C isotherm in which they observed no intermediate phases, and on which they established the limits of solubility as 36.5 at. pct W in ruthenium and about 1.5 at. pct Ru in tungsten. In addition, Obrowski2 found a o phase forming peritectically from the melt and existing only above 1650°C. Below this temperature the phase was presumed to decompose eutectoidally. The present work finds the diagram as given in Fig. 1. I) EXPERIMENTAL PROCEDURE The materials used for alloy preparation in determining the W-Ru constitution diagram were 99.9 pct pure ruthenium powder supplied by Baker Chemical Co., and 99.9 pct pure tungsten powder from General Electric Co. Typical analyses of these elements are given in Table I. Initial alloys at 10 at. pct intervals were prepared from the metal powders by the following method. Powders sufficient for 25 g of the alloys were weighed out with an accuracy of 0.1 mg and blended mechanically. After blending, the powders were compacted, in a steel die, at approximately 30,000 psi. The compacts were sintered in an electric vacuum furnace in order to remove adsorbed gases and to achieve partial densification prior to arc-melting. Vacua of 10-4 mm Hg or less were maintained in sintering as the furnace temperature was raised to approximately 2000°C. Sintering times ranged from 10 to 20 hr. The sintered compacts were arc-melted under a protective atmosphere of purified helium. Melting was conducted on a water-cooled copper hearth, utilizing a nonconsumable tungsten electrode. In the melting process, each alloy was turned over and re-melted on opposite sides from four to six times to ensure complete melting and to eliminate gross in-homogeneities. The arc-melter used had a vacuum capability of 5 X 10-6 mm Hg, and a leak rate of about 20 -liters per hr. Chemical analysis techniques for refractory metal-platinum group metal combinations are not well-established; therefore, composition control and determination depended principally upon weight-loss observations and calculations. This consisted in weighing each alloy after sintering and after arc-melting, and calculating the maximum and minimum composition values, assuming the total weight losses to be first all tungsten, and then all ruthenium. Since composition uncertainty was directly related to weight loss, care was taken to minimize losses in handling, compacting, and melting. Prior to homogenization and equilibration the as-arc-melted alloys were analyzed in several

Jan 1, 1964

By G. R. Purdy, J. G. Parr

The intermetallic compound Ti2Co was studied by X-ray diffraction and metallographic techniques. The phase occurs off stoickzometric composition, with its greatest variance at high temperature. The solubility limits of the phase have been cletermined, and an amendment to the titanium-cobalt phase diagram is suggested. THE first intermetnllic compound to appear at the titanium-rich side of the titanium-cobalt system was found by Laves and wallbauml to be Ti2Co. They described this compound as isomorphous with Ti2Ni and Ti2Fe, and demonstrated that it had a face-centered-cubic structure with 96 atoms per unit cell. This contention is supported by the work of Duwez and Taylor2 and Orrell and Fontana3 who also determined the lattice parameter to be about 11.30A. Rostoker4 believed that Ti2Co did not exist, and that the phase considered by the other workers to be Ti2Co was Ti,Co20. However, Orrell and Fontana determined oxygen and nitrogen contents and found that their alloys did not contain sufficient of these elements to produce significant quantities of a stoichiometric oxygen compound. The present investigation was initiated to determine the composition limits of the phase Ti,Co.

Jan 1, 1961

By R. Wachtell

IN order to study better the phenomena at work in various phases of diffusion of the Fe/Si system when compounded and alloyed by powder metallurgy methods, several attacks have been planned. Electrical, hardness and other measurements have been discussed e1sewhere.l,2 The metallographic phenomena will be considered here. Concerning the metallography of the ferrosilicon alloys, some initial discussion is in order. As this laboratory discovered to its chagrin, there are many traps that lie in wait for even the experienced metal-lographer when he deals with alloys of high silicon content. Chief of these is probably the anomalous behavior of these materials under conventional etching techniques. We have before us, for instance, Corson's paper" of 1928, wherein is mentioned and illustrated (probably for the first time) the peculiar "barley shell" structure sometimes found in these alloys. Again in 19412 he same author reports the structure in 5-14 pct silicon irons. Houghton and Becker mention its presence' but make only tentative effort to explain it. In 1943, Hurst and Riley6 discussed the "barley shell" and declared it to be a false structure, resulting from the peculiar and characteristic film-forming propensities of the alloy. At about the same time, Wrazej7 proved correct the contentions of Hurst and Riley, establishing pretty well the mechanisms of formation and identifying the constituents involved. Hurst and Riley6 a1so describe in their paper (1943) a "cracked film" structure, also a pseudo-morph, the precise nature of which they do not suggest. Careful examination of such a film reveals that it not only cracks but begins to curl away from the surface of the metal and peel, much in the manner of flaking paint. The careful microscopist will be able to focus on the topmost edge of the flake, and, by optical sectioning, follow it down to the metal surface. We have been able, by oblique illumination of such specimens, to observe the raised segment of the film, the shadow that it casts, and the mating segment on the metal into which it fits. As late as 1946, Hurst and Riley8 found occasion to correct misinterpretation of this "cracked film" structure in a work by others on a 12 pct Si/Fe alloy. The "barley shell" and "cracked film" pseudo-morphs are not the only ones encountered in studies of these materials. A third pseudomorph, which may, however, have some structural significance is a fine striation of the surface. Closely spaced and parallel striae extend entirely across single grains. Each grain shows a different direction for the striae, and different closeness of the spacing. The regularity of this structure, and the fact that the striae do not cross from one grain to another, suggest that the structure is a film cracking controlled in some way by the crystal plane orientation of the surface being etched. In general it is wise for the metallographer dealing with these alloys to cultivate a feeling of uncertainty not only of the more complex questions of interpretation, but also of the basic question of whether that which he sees is indeed a true representation of the structure. We have taken, as a first test of the validity of a structure, its reproducibility "in situ" after repolishing and re-etching of the samples. Thus we knew the "barley shell" to be false (fig. 1) even before encountering the definitive works on the subject. The Metallography of Silicon Diffusion in Laminate Bars: As a first step in the study of the metallography of the diffusion process, we have pressed a series of laminate bars. These bars, or "sandwiches" as we have termed them, were pressed with covering layers of iron powder, and a "filler" of the Fe/Si master alloy under study. Bar dimensions were approximately %, x 3 x 1/4 in. The total

Jan 1, 1951

APRIL BEGAN with increased disorder in the Ruhr and some blood-shed. The war cloud in the East disappeared, however, with the signifi- cance by the Turks of their intention to return to Lausanne to negotiate a treaty of peace with the Allies. The French occupation of the Ruhr continued during April without there being any spectacular develop-ments. Of course there was surliness on the part of the Germans. In the meanwhile the statesmen on both sides were intimating what they might give and what they might take, sounding the sentiment of their respective populaces. The British Government found that its revenue for the last fiscal year has been greatly in excess of expenses. The surplus was applied to reduction of the debt. A consequence of this development has been a reduction in British taxes for the ensuing year, which has naturally created a much better feeling in Great Britain. On the other hand the unemployment situation in Great Britain caused increasing alarm. At the begin-ning of April about 1,500,000 men were out of work and the thought was developing that this might be not merely a temporary emergency, but a long continuing condition. The uneasiness of the workers themselves began to be exhibited in increasing strikes and threats of strikes. There were important domestic events during April. The six miners who were on trial in Illinois for the Herrin massacre were acquitted, following which the State dropped further prosecutions on the ground that Williamson County is so thoroughly under labor domina-tion that justice could not be had there. The Supreme Court of the United States on Apr. 10 handed down a decision that an act of Congress fixing minimum wages for women in the District of Columbia was unconstitu-tional, being interference with the freedom of contract included within the guarantees of the fifth amendment. Advances of wages became more general during April. The leading event under this head was the action of the United Steel Corporation putting into effect an.11 per cent. increase in the wages of common labor on Apr. 16, by virtue of which the rate per hour was raised from 36 c. to 40 c. This was dictated by competitive conditions, the labor difficulties of the steel industry being due less to a scarcity of men than their disinclination to take jobs in that industry while the building and other industries were paying as high as 60 c. per hour for similar work.

Jan 5, 1923

By Samuel G. Lasky

What the evidence prevails upon the mind to believe, depends upon the mind as well as upon the evidence. M. L. IN a recent discussion of the mineral resource position of the United States, published in the September 1946 issue of MINING AND METALLURGY, I expressed my conviction that ore deposits of major magnitude remain to be found in this country and that they can be found without undue cost or risk. I stated with equally strong conviction, however, that if the search for such deposits is to be notably successful there must be, among other things, a reorientation of philosophy and mental habits on the part of many who would be connected with the search. I would now like to enlarge upon that statement. For such a purpose, we may consider that the search for concealed deposits involves four steps: (I) the selection of areas for further study; (2) the geologic study of those areas in order to verify their general favorableness and in order to choose specific patches worthy of being tested; (3) the decision whether exploration of the patches chosen should actually be undertaken; and (4) the exploration itself. The first two steps and the last rest upon the judgment and skill of geologists. The third step-the decision whether exploration should be undertaken-rests upon management. In my opinion, the philosophies or principles that have guided these steps in the past are now inadequate. PHILOSOPHY OF APPRAISAL If concealed deposits are to be looked for, how are the places of their possible concealment to be recognized? Every known mineralized area still in the prospect stage has already been repeatedly examined and condemned. As for those deposits concealed under later rocks, there may be not even the clue of a near-by outcrop for engineer or geologist to consider. How then, are we to know where to look? Geologic Probability In the early days of our mining industry, ore deposits were found mainly by "following the ore." Later, as such opportunities decreased, and as geologic concepts became accepted, deposits were found more and more through use of the notion of geologic probability. Many instances can be cited wherein a courageous operator ignored the implications of the unsuccessful efforts of predecessors and, solely by "following the ore," converted a discredited prospect into a good mine. Similar experience doubtless will occur in the future, but "following the ore" will no longer in itself find new deposits in the amount needed. Nor can enough new ore be expected from further use of the notion of geologic probability, for, as mentioned above, our known prospects `have already been ex-

Jan 1, 1947

Prof. J. W. Richards, South Bethlehem, Pa. (in reply to several questions):—The cut representing some of the round briquettes which were under test shows that, at the brcaking-stresses, they break into lumps, and do not disintegrate into powder. The process is simplicity itself. I have followed the different processes for sintering iron-ores and flue-dust, am interested in all of them and wish them all success; but this process appealed to me strongly by its simplicity. It is in line with a method which I once tried to work out myself, but which never came to anything, namely, the agglomeration of fine iron-ores by means of Portland cement. As small an amount as 5 or 6 per cent. of Portland cement will enable fine ore to agglomerate and set into a briquette, but when I came to estimate the cost, I found it was a little too high. The Schumacher process, curiously enough, does not work well on iron-ore, but flue-dust thus treated does harden and give a strong briquette. In my attempts to find a reason for this difference, it has occurred to me that possibly the particles of flue-dust had been coated over with some sublimed silica, which might be an agent in the setting. But I found by experiment that neither sublimed silica, nor ordinary silica, nor ordinary alumina, would briquette. Chemically pure iron oxide briquetted quite hard; but the application of pressure is a necessary part of the operation. If simply moistened with the solution and allowed to stand it does not set hard, but the more pressure applied to it the hardcr it sets. Evidently the flue-dust particles must be pressed very close together in order to get the small proportion of active material wet, so that the particles shall act at their points of contact; for it is evident that only at the points of contact does the cementing action take place. The reactions are facilitated by considerable pressure, bringing the acting particles close together, and may go on with

Jan 1, 1913

By A. F. Crawley

The densities of some liquid Pb-Sb alloys up to 11 wt pct Sb and Pb-Sb-& alloys up to 10 pct Sb/10 pct Sh have been determined by a pycnometric technique over a temperature range of about 130°C above their melting points. The data given are accurate within 0.05 pct. Density is shown to vary linearly with temperature , and equations relating these quantities have been formulated. Molar volumes calculated from the density data indicate that volumetric deviations from ideal mixing are undetectable within the limits of experimental error. A continuing research program into some fundamental physical properties of liquid metals is being pursued at the Mines Branch, Department of Energy, Mines and Resources, Ottawa, Canada. This work has received support from the Canadian Zinc and Lead Research Committee in cooperation with the International Lead and Zinc Research Organization. This paper, which reports some density data for Pb-Sb and Pb-Sb-Sn alloys, follows previous work from this laboratory on lead, tin, and Pb-Sn alloys.' Of previous data from others, Greenaway2 and Sato and Munakata3 have reported results on Pb-Sb alloys. No previous work has been published on the ternary Pb-Sb-Sn alloys, reported here. EXPERIMENTAL METHOD Densities were measured by a pycnometric technique which has been described in detail and appraised for accuracy in earlier Mines Branch reports.475 Fig. 1 shows the densitometer with the pycnometer in position for a run. The pycnometer is also shown in some detail. The pycnometer of dense, high-purity graphite, about 14 cu cm in volume, was carefully machined to a uniform, smooth finish. The height was measured by a depth micrometer and the diameter by fitting precision gage blocks between steel balls.' In each case several readings were taken, and the final results were considered accurate within 0.01 pct. The resulting volumetric uncertainty together with small inaccuracies in the coefficients of linear expansion of graphite lead to a maximum systematic uncertainty in the method of ±0.03 pct. As shown in Fig. 1, the pycnometer lid is a threaded cap. Thus, the charge, a cylinder of the alloy, can easily be inserted and the solidified metal can readily be removed after a run. The dimensions of the cylindrical charge are chosen to ensure that, once molten, the metal will not only fill the pycnometer completely but will discharge an excess into the excess-metal float chamber. AS the temperature is increased above the melting point, the volume of metal in the excess chamber increases until the system has equilibrated at the desired temperature. At this point, the excess chamber is moved to one side by twisting the shaft F, leaving a fixed volume of liquid metal in the pycnometer. This volume of fluid is readily calculated using measured coefficients of linear expansion of the graphite which expands anisotropically. The associated weight of fluid is determined as the weight of the solidified metal removed after the furnace has cooled down. Alloys were prepared from 99.997 pct Pb, 99.999 pct Sn, and 99.999 pct Sb, being melted by an electric furnace in a graphite crucible and poured into graphite molds. Several density specimens of the same nominal size were machined from each ingot, and, by comparing specimen weights, relative differences in specimen composition resulting from segregation in the ingots could be detected. In this way, segregation was found to have occurred in Pb-Sb alloys at compositions beyond the eutectic (11.2 pct Sb) and this

Jan 1, 1969

By Harold L. Overton, Leonard B. Lipson

The first paper in this series1 outlined practical methods for applying the theory of steady-state flow of an ideal Bingham plastic liquid through a circular pipe and axially through a stationary concentric annulus to the enginekring analysis of friction loss problems. In the present paper the properties of another useful rheological model, the pseudoplastic generalized Newtonian liquid, are considered. The terminology applied to the rheological models is derived from the following classification of rheological models. The term "generalized Newtonian" is a class designation applied to models which do not have yield points but which exhibit a dependence on shear rate. The term "pseudoplastic" applies to a sub-group of models within this class which exhibit a decrease in "viscosity" with increasing shear rate. The term "power model" refers to a mathematical model proposed for describing the behavior of the pseudoplastic liquid. This model is of interest since certain of the salt saturated, oil emulsion, and "low solids" drilling fluids, inverted emulsion- and oil-base drilling fluids, aqueous gels, gelled crudes and blocking agents employed in hydraulic fracturing operations are of this type. The present treatment considers the equations describing steady-state Poiseuille flow through a circular pipe and a stationary concentric annul us, and Couette flow between concentric rotating cylinders for a particular pseudoplastic model. As in the previous paper' it is demonstrated how these equations can be applied to engineering calculations of friction losses. Graphical procedures for recovering the various flow curves and cxample calculations are included. A method for simplifying turbulent-flow correlations is also proposed. PROPERTIES OF PSEUDOPLASTIC GENERALIZED NEWTONIAN LIQUID In contrast to the Bingham plastic the generalized Newtonian liquid is yield point-free. However, in the flow region the relation between stress and rate of shear is not linear as it is with ordinary Newtonian fluids. If the stress increases with shear rate at a less than linear rate the system is called pseudoplastic. While there is no yield point in this system, the Bingham advocates' coined the term pseudoplastic to distinguish this kind of behavior from Bingham plastic behavior. For the pseudoplastic a plot of flow rate vs friction loss or rpm vs torque, from pipe flow or rotational viscometer measurements, respectively, generally has three qualities: (1) it can be clearly extrapolated toward the origin; (2) there is very little slope at the origin. This accounts for the high apparent viscosities at low mixing and pumping rates; and (3) the flow curve possesses a continuous curvature which gradually diminishes as the shear increases. Rheological measurements on a pseudoplastic liquid can be easily misinterpreted as indicating Bingham plastic behavior. A typical case in point is illustrated in Fig. 1. These data were obtained from measurements on an oil-emulsion mud using a commercially available rotational-type viscometer (Model 35 Fann V-G meter). Applying the "two-point"* method3 gives a plastic viscosity of 17 cp and a yield point of 24 lb/100 ft2; at the same time weighting material settles very easily in this system. This illustrates that it is not possible to distinguish between the pseudoplastic and the Bingham plastic from only two data points. It is possible to determine qualitatively which model is more appropriate by a combination of dynamic and static measurements. Experience indicates that the simplest criterion for the Bingham plastic liquid is that the calculated dynamic yield point should be of the same magnitude as the measured gel strengths. For the oil-emulsion drilling fluid illustrated in Fig. 1, a value of 4 lb/100 ft2 was obtained for gel strengths measured

By D. D. Porter, H. G. Carlevato

Blasting to prepare orebodies for in situ leaching usually involves extraordinary conditions which sometimes require special and innovative techniques. To date several unusually large blasts have been made for leaching with results that are very encouraging. Among the factors considered when designing these large blasts are orebody shape and depth, rock properties, vibration and damage potential, loading logistics, and safety. All of these factors, and others, are discussed with an effort made to put each of them into its proper perspective.

Jan 1, 1974

By T. Egleston

The origin of gold both in placer deposits ancl in veins, and especially the origin of nuggets, has been the subject of repctated discussions and investigations, which have been recently brought to my attention by several extremely interesting specinlens sent to me for examination, and mare especially by the one exhibited at the meeting of the Institute in February, 1880.* In the year 1874 I made some exan~inations of the hydraulic mines of California, and was very nluoh struck with the distribution of the gold throughout these deep placers, which were almost invariably poor on'the surface, while gradually growing richer towards the bedrock. The constant presence of fossil wood, and the large quantity of organic matter contained even low down in these beds, was also remarkable. Not being satisfied with the various theories advanced to account for the formation of these deposits, I began an investigation early in the pear 1879 on the conditions of solubility of gold and the causes of the loss in working gold ore in a large way. The researclles which I have undertaken show that gold must be considered a soluble rather than an insoluble metal, and that the conditions of solution are such as will be found anywhere where gold is likely to occur, and the solution may take place even under the ordinary circumstuncee of surfiace drainage, and may be going on freely even where the presence of gold has never been suspected, and that there are causee enough in nature to produce the solution of the gold in sufficient quantities to account for all the phenomena of both the vein and placer formations. The general theory with regard' to the formation of these placer deposits and nuggets has been that they were the result of the deatruction of pre-existing. vein-matter, which does not accord with the fitcts as sholvn in the deep placer deposits. The gold in such case would be distributed in layers of unequal richness throughout

Jan 1, 1881

By J. Richter, D. Schulze

J. Richter and D. Schulze (Deutschen Akademie der Wissenschafte zu Berlin)—Introduction. In a recent paper R. G. Garlick and H. B. Probst reported on experimental results of investigations of room-temperature slip in zone-melted tungsten single crystals.17 In the paper it was pointed out that slip lines could be detected with an optical microscope only after about 10 pet plastic strain of the crystal. In our investigations we could observe slip lines in tungsten single crystals of defined orientations already with an elongation of 0.02 to 0.03 pet.18"9 Experimental Technique and Results. The tungsten single crystals were produced from 4 to 5 mm sintered rods* as starting material by electron- beam zone melting. With single-zone-pass melting a speed of 0.5 mm per min was used, while three-pass melting could be handled at a speed of 3 mm per min. Crystal axis orientations were located in the shaded area of the stereographic triangle, see Fig. 6. Orientation 1 is located at about 18 deg and orientation 2 at about 5 deg on the great circle from [011] to [ill]. This corresponds approximately to the orientations P and M referred to by Garlick and Probst. Our single crystals had a length of about 70 mm and were profiled solely by electrolytic means, leaving grip ends at both ends of the crystals. Between the latter, a cylindrical crystal of 45 to 50 mm length and about 2.4 mm diam was obtained. The crystals were deformed at room temperature in a commercial tensile-testing machine to obtain a strain of 0.02 to 5 pet. The average strain rate e = eP/t for all tensile tests amounted to approximately 10 -6 to 10-5 per sec, with ep representing plastic strain and t the duration of applied stress. In Fig. 7 a crystal is shown elongated by 0.03 pet. The picture was obtained by means of an optical microscope. Figs. 8 and 9 give electron-microscopic pictures of slip lines of crystals elongated by 0.07 and 1.1 pet, respectively. For crystals with the orientation 1, see Fig. 6, only the two main slip systems (101)[111] and (110)[111] were found. With the crystals of group 2 the two main slip systems are again evident, with

Jan 1, 1965

By P. H. Thornton

MaNY intermediate phases are solid solutions which have a solute-solubility range greater than 3 at. pct. These phases, which are generally very strong and often have simple crystal structures, are usually extremely brittle so that specimens of simple shape cannot be produced by the usual mechanical-deformation techniques. Furthermore, single crystals of reasonably uniform composition are difficult to grow by the Bridgman technique because the phases generally form by a peritectic reaction, which causes pronounced segregation. In this note, a technique is described for the preparation of thin-rod specimens of brittle intermediate phases, which may be used for physical-property studies such as resistivity changes' and for the conversion of such rods into single crystals. The method has been used for the preparation of rod single crystals of the phases and Ingots, of about 100 g weight and 11 mm diam, were made by melting together the appropriate amounts of high-purity materials (usually 99.999 pct) in sealed

Jan 1, 1967

By R. B. Sosman, J. C. Hostetter

It is well known that ferric oxide, Fe2O3, is paramagnetic, while magnetite, Fe3o4, is classed among the highly ferromagnetic substances. But magnetic data on oxides intermediate in composition between Fe2o3 and Fe3O4 have been almost completely lacking. Fe2O3 and Fe3O4 form a solid-solution series, according to present evidence.' In this series the properties change continuously from Fe2O3 toward Fe3O4, as the percentage of FeO increases from zero toward 31.03, which is the percentage in magnetite. It is possible that there is a break in the series near Fe3O4, but it has not yet been possible to establish the existence of such a break experimentally. The occurrence of solid solution in this series is shown by the dissociation pressure, or oxygen pressure in equilibrium with the oxides, which falls continuously over the range from Fe2O3 to Fe3O4. The oxygen-pressure curves at 1100" and 1200" are shown in Fig. 1. The existence of solid solution is also demonstrated by the continuous change in optical properties from Fe2O3 over to a composition containing about 18 per cent. FeO, at which point the opacity of the oxide becomes so great that it is impossible to obtain measurements at higher percentages of ferrous iron. Natural oxides of iron intermediate in composition between Fe2O3 and Fe3O4 are much more common than is generally supposed. If a mineral oxide is not strongly attracted by a small hand magnet and if it gives a red streak, it is usually labeled "hematite." If it is strongly attracted by the hand magnet it is usually labeled "magnetite" without further tests. As we shall show later, oxides containing from 1 up to 31 per cent. FeO can be thus erroneously lumped together as "magnetite." It is a fact, nevertheless, that the great bulk of natural oxides of iron lie fairly near either Fe2O3 or Fe3O4 in composition. The reason will be

Jan 1, 1918

By Ray W. Ballmer

"For his leadership in developing and managing large, complex, and technically innovative mines, particularly the outstanding and successful Bougainville mine and for his lecture, 'The Moving Targets of Mine Development '. " Recipient of the 1981 D. C. Jackling Award

Jan 1, 1982

By M. E. Straumanis, J. -P. Krumme

In basic ([KOH + KCl] with a total polarity of 2) or acidic (2N H2SO4) electrolytes and at anodic current densities of more thun 2 to 4 ma per sq cnz, n-type GaAs single crystals of lozo resistivity preferentially dissol~je forming etch tunnels with triangular or civc~ilay cross sections and of a width between 0.5 arid 5 p. These etch tunnels are oriented along any one of the four possible (111) directions of GaAs. However, their growth occurs only in one direction of a given (111) whick apparently is determined by the atomic sequence Ga —As (and not the rezlerse) in respect to an individual valence bridge in the crystal. It is concluded from comparison with the cubic lattice structure of GaAs that the etch tunnels represent macroscopic evidence for the tetrahedral bonds and their polar properties. If the anodic current density is increased the tunnel fomation results in the development of a fibrous surface layer consisting of GaAs. The latter separates frorn the substrate (in an anodic s~irface disintegration process) by the growth pressure of an As,0, filnz forming in the interior of the fibrous layer, 100 to 200 µ under the surface, at more than about 50 ma per sq cni. The fibrous GaAs film has the same crystallographic orientation as the substvate and represents a skeleton of the original crystal. Since the etch-tunnel density in a separated GaAs layer is about 108 c?n-', and the etch tunnels develop only along (111) in a given polar direction, it is assurraed tlmt the dislocations have no influence on the growth of these tunnels. ElECTROLYTIC treatment of smooth surfaces of poly- and single-crystalline GaAs at high anodic current densities causes the formation of porous surface layers.' This phenomenon suggests comparison with effects being observed with magnesium,' indium,, gallium,4 and aluminum5 and known as "anodic disintegration". The purpose of the present paper is to explore and to explain the reasons for the formation of such surface layers on GaAs and, in particular, to investigate the influence of the lattice polarity of this III-V compound semiconductor in the (111) direction on the anodic dissolution behavior. GaAs SINGLE CRYSTALS For the experiments described below GaAs single crystals from the Monsanto Co., St. Louis, Mo., were used. Their impurity levels were below 1 ppm and their dopant levels between 1 and 100 ppm. They were grown in (111) using the Czochralski or the gradient-freeze technique. The crystals had n-type conductivity and electric resistivities between 1 and 5 ohm-cm. EXPERIMENTAL The GaAs single-crystal rods were cut perpendicularly to (111) into wafers of about 1 mm thickness using a wire-blade crystal slicer and an aqueous slurry of Sic or a diamond saw. The orientation of the faces of these wafers were checked by Laue back-reflection patterns. If there was a deviation from (111) the faces were abraded under a certain angle using grinding paper and distilled water. The damaged surface layer was removed from each crystal by chemical etching with a mixture of 1HF:1HNO3: 1H20 or 2HF:1HNO3:2HAc (glacial). {110) faces were obtained by mechanical cleavage, producing surfaces which did not require a further treatment. The GaAs wafers were mounted using "alligator" clamps instead of soldered electrical contacts.' Only the bare crystal surfaces were dipped into the electrolyte. The clamps were coated with insulating wax to prevent any contact with the electrolyte. The experiments were carried out in aqueous 2 N H2so4,' or in an aqueous solution of KOH and KCl1 (1 mole KOH + 1 mole KCl in 1000 cu cm solution). Anodic current densities up to several hundred ma per sq cm were applied for periods between 30 sec and 2 hr. For the purpose of investigating the initial steps of disintegration the anodic current density applied never exceeded 20 ma per sq cm. The films which partially separated from the anodic surfaces under high-field conditions were treated with KOH to further their detachment by dissolving the As2O3 formed. The washed and dried films were pasted to strips of filter paper, and Laue pictures were made. The back-reflection patterns obtained were compared with those of the original anode surface before and after anodic dissolution. Furthermore, space reciprocal lattices7 were constructed from asymmetric rotation crystal patternsa which permitted the determination of the crystallographic orientation of the detached films of the corrugated anodic surfaces. The disintegration products were identified from assymmetric powder patterns.8 The polarity of the {111) faces was determined by chemical etching with mixtures of 1HF:1H2O2(30 pct): 2H2O or 1HNO3:2H2O. Different patterns on each of two inverse (111) sides appeared.'-l8 The correlation of these patterns to the Ga{111) or the As(111) side has already been established by the use of light figures,18-20 by X-ray diffraction near the absorption edges of gallium and arsenic,'lmZ4 and by LEED measurements.25 The geometric structure of these surfaces and the interior of the anodically attacked crystals were observed and photographed with a high-power microscope using oil immersion objectives up to magnification of X1720.

Jan 1, 1968

By A. N. Roberts, N. W. Stump

New developments in on-stream analysis using immersed radioisotope gages including results from plant installations are described. The control of grinding and flotation using a small digital computer has been complemented by this development. A control scheme for grinding, which is based on maximum throughput at constant product size, and preliminary work in flotation control are also outlined.

Jan 1, 1975

By F. W. Schroeder

AT the annual meeting of the Institute 2 years ago, a paper,1 " Requirements of Refractories for Open Hearths," was presented by F. W. Davis and G. A. Bole of the U. S. Bureau of Mines. In a brief foreword, D. A. Lyon stated that the paper was not to report the results obtained but rather to present an outline to serve as a basis for discussion. The essential parts of an open-hearth furnace were described and the conditions under which they operate. Some constructive discussion followed the reading of the paper. One of the first fellowship investigations undertaken by the Bureau of Mines in 1924 under the cooperative agreement with Carnegie Institute of Technology, through the Metallurgical Advisory Board, was to determine service conditions of open-hearth refractories. The present paper gives the results of this work which was done in the Pittsburgh district and was in charge of the authors. Material contributions in the form of data were contributed by E. N. Bauer, J. W. Campbell, G. H. Pfeiffer and A. Grodner, Carnegie Institute of Technology research fellows. The study covered 18 mos.

Jan 7, 1926

By E. Lancaster-Jones

THE gravity magnitudes obtained by means of observations with the Eötvös balance in the field are necessarily resultant or total effects due to all abnormalities of mass distribution, including even the effects due to the ellipticity and rotational motion of the whole earth. Since the object of the survey is to isolate the effects which arise solely from some particular subterranean feature, and to deduce therefrom the configuration and extent of this feature, the first step is to eliminate from the observed effects all those due to "disturbing" (i. e., unwanted) features, whether above or below the surface of the ground. The disturbing features have different characteristics, according to their situation relative to the center of the balance and to the horizontal plane through the foot of the balance, or station point; this diversity was recognized by Eötvös, who divided the total effects into so-called Normal, Terrain, Topographical, Cartographical and Subterranean effects. This classification has been adhered to by most subsequent investigators, but the writer prefers to employ the term "three-dimensional," which really indicates the essential character of the class of effect known as "Subterranean," at any rate from the standpoint of the computer of effects. Before disturbing effects can be eliminated, the features must be measured up or surveyed, whether by topographical, mining, or boring methods, and then the effects of each feature calculated and subtracted from-the total observed effects. After this the problem of interpreting the residual effects will itself necessitate the computation of the assumed feature, or even a series of trial features.

Jan 1, 1928

By E. Lancaster-Jones

THE gravity magnitudes obtained by means of observations with the Eötvös balance in the field are necessarily resultant or total effects due to all abnormalities of mass distribution, including even the effects due to the ellipticity and rotational motion of the whole earth. Since the object of the survey is to isolate the effects which arise solely from some particular subterranean, feature, and to deduce therefrom the configuration and extent of this feature, the first step is to eliminate from the observed effects all those due to "disturbing" (i. e., unwanted) features, whether above or below the surface of the ground. The disturbing features have different characteristics, according to their situation relative to the center of the balance and to the horizontal plane through the foot of the balance, or station point; this diversity was recognized by Eötvös, who divided the total effects into so-called Normal, Terrain, Topographical, Cartographical and Subterranean effects. This classification has been adhered to by most subsequent investigators, but the writer prefers to employ the term "three-dimensional," which really indicates the essential character of the class of effect known as "Subterranean," at any rate from the standpoint of the computer of effects. Before disturbing effects can be eliminated, the features must be measured up or surveyed, whether by topographical, mining, or boring methods, and then the effects of each feature calculated and subtracted from the total observed effects. After this the problem of interpreting the residual effects will itself necessitate the computation of the assumed feature, or even a series of trial features.

Jan 1, 1928

ON JUNE 7 the German Government handed to the French and Belgians a new proposal for reparations, which offered 1,200,000,000 gold marks annually, to be guaranteed as to 500,000,000 by a mortgage on the national railways, as to another 500,000,000 by a mortgage on industry, commerce, land and factories, and as to 200,000,000 by a luxury tax. The number of years for which this payment should run to be left to settlement by an international conference. This offer was taken under consideration by the French and Belgians, who instituted conversa-tions with the British in the hope of arriving, at some joint action with respect to the Germans. Up to the end of June nothing had been determined. In the meanwhile, the continued French and Belgian occupation of the Ruhr seemed to develop a condition of guerilla warfare, considerable bloodshed occurring throughout the region. The second Lausanne Conference dragged on, the Allies being apparently unable to take any firm, joint stand, while the Turks increased their importunities and managed to get concession after concession. Early in June a revolution occurred in Bulgaria, the previous Government under Premier Stambulisky, based on the agrarian party, being forcibly thrown out by a bourgeois and military combination. This pro-duced considerable disorder in Bulgaria, outside of which country the nature and purpose of the revolution does not appear to be well understood. Stambulisky's partisans offered feeble, isolated resistance to the revolu-tion; in connection with which there was some blood-shed and Stambulisky himself was reported killed, although this was later contradicted. Professor Zan-kof, the new Premier, issued a statement, that the change of the Government was the result of discontent, that the foreign policy of the new Government would be peaceful, and that Bulgaria would continue to fulfill her international obligations, particularly the treaty of Neuilly. It was the opinion of London that the immu-nity from taxation enjoyed by the farmers under the agrarian regime is likely to he superseded by more equi-table taxation, and in general that the bourgeoisie will be better administrators of the public affairs In domestic affairs industrial activity continued at a high rate, but there was distinct relaxation in the demand for raw materials, and also in some manufac-tured goods. During June there were reductions of prices by many of the automobile tire manufacturers. There seemed to be also further contraction in the demand for automobiles.

Jan 6, 1923