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By F. O. Shuck, F. E. Butler

A diaphragm diffusion cell suitable for use with liquid metals was designed and tested by measuring the diffusion coefficients for a Hg-10 pct In alloy at 25°C. The binary diffusion coefficient and the coefficients for In and Hg tracers were measured at this composition. The measured coefficients for both tracers were less than the binary diffusion coefficient. When these coefficients were combined with the activity correction term of Darken, the predicted binary coefficient was somewhat higher than the experimental value. In recent years a number of investigators have been studying diffusion of liquid metals in order to gain a better understanding of the liquid state and to examine possible applications to liquid metal processing. The bulk of this work has involved either self-diffusion or diffusion of low concentrations of solute metals in an essentially pure solvent metal. The most common experimental technique employed has been the capillary-reservoir method of Anderson and saddington1 since it is well-suited to measurements involving low concentrations of solutes. As an expansion of previous studies, an investigation of the variation of diffusion coefficient over large composition ranges has been undertaken in this laboratory. Although it is possible to modify the capillary-reservoir method for such measurements, the technique loses its principal advantage of requiring only small quantities of solutes. Therefore, it was felt desirable to investigate other possible experimental techniques applicable to measurements over large composition ranges. A technique which has been used widely in measurements of other liquid systems and seemed potentially applicable to studies of liquid metals was the diaphragm cell. This method has been found to combine relative simplicity of operation with accurate and reproducible results. In use with normal liquids, the tyiical diaphragm cell utilizes a porous glass disk. However, because of the high surface tension, it is not possible to use a diaphragm of such fine pore structure with liquid metals. Furthermore. projected use at high temperatures makes the use of glass undesirable. Consequently, the first problem was the search for an appropriate cell design. EXPERLMENTAL Diaphragm Cell. A number of possible cell designs were examined. Prototypes of several were constructed and tested. The final design is shown in an exploded view in Fig. 1. The cell consists of two identical chambers, one on either side of a 0.20-in.-thick partition. The chambers are 0.15 in. deep and have a volume of 3.45 cu cm. Each chamber is provided with two small threaded holes for filling and emptying. The filling holes may be sealed with stainless-steel screws. Drilled lengthwise through the center partition is a 0.250-in.-diam hole. Inserted into this hole is a rod having seven 0.059-in.-diam holes drilled radially through it. The total "hole" volume is 0.078 cu cm. When the rod is properly aligned, the holes in it constitute the "diaphragm" through which diffusion occurs. The center section was of Teflon and the rod and face plates were of Plexiglas. Four such cells were constructed and used in this study. Subsequent to this investigation, a similar cell constructed entirely of iron was fabricated and tested at higher temperatures. Several considerations led to this final design. It is desirable to minimize the volume of the cell chambers to decrease the time required for a measurement. However, the total volume of metal in the diaphragm must be small in comparison with that in the chambers. To facilitate filling and emptying it is desirable to have a diaphragm which may be closed.

Jan 1, 1970

By T. E. Seidel, A. U. MacRae

The dependence of the electrical and crystalline properties of silicon containing ion implanted boron atoms have been studied as a function of the incident dose, substrate temperature, and annealing tempera-ture. Hall effect studies show that the compensation due to defects is negligible after annealing at and above 500°C for a dose of 1013 ions per sq cm. Steps occur in the isochronal annealing curve for the sheet resistance at 300°C and 800°C and the mechanisms responsible for these steps are discussed. The range of the ions at 150 kev is 3500 * 5001. Electron diffraction studies on samples implanted with 150 ker ions show the existence of damaged (polycrystalline) silicon closer to the surface than the range of the ions. Etching and subsequent annealing of etched and unetched specimens suggest that the poly crystalline silicon is closer to the surface than the bulk of the distribution of ions. THE purpose of this study is to investigate some electrical and crystalline properties of ion implanted boron in silicon. Sheet resistance, Hall measurement, depth distribution by chemical staining, thermal probe and electron diffraction have been used to study the properties of samples implanted in a random direction with ions having energy up to 150 kev. The boron-silicon system has been the subject of considerable study'-7 due to its possible application in the fabrication of electronic devices. The implanted ions produce considerable crystalline damage to the substrate crystal before they lose most of their primary energy and come to rest. Fortunately, most, if not all, of this damage can be removed by subsequent annealing or by holding the substrate at an elevated temperature during the implantation process. Sheet resistivity measurements of the p-type layers produced by boron implantation into room-temperature silicon, reveal that the annealing occurs in a two-step process: the first occurring at -300°C and the second at -800°C.' Electron-microscope and low-angle electron diffraction studies of this damaged material indicate that the bombarding ions produce an amorphous silicon region about the trajectory of each ion.' At high doses, these damaged regions overlap and an amorphous surface layer results. Furthermore, the 800°C annealing step, appears to be associated with the elimination of this gross damage. The depth distribution of the as-implanted and also the annealed samples have been studied by an angle lap and staining technique as well as by Hall measurements.3-7 We find the experimentally determined ranges of the boron are less than those calculated by the Lindhard-Scharff-Schiott theorys (hereafter referred to as the LSS theory). Our results are in essential agreement with pre- vious results. In addition, we have made Hall measurements on samples bombarded with a low dose (2 x 1013 ions per sq cm) to minimize impurity banding effects, and find that deep ionized levels influence the carrier concentration and room-temperature hole mobility until the sample is annealed at temperatures above 500°C. Above this temperature, the data corresponds to that obtained when silicon is doped with boron by conventional techniques. We have also made a depth distribution determination of the crystalline damage due to the implanted boron by using glancing angle electron diffraction techniques. It was found that the gross damage depth distribution of heavily implanted samples is closer to the surface than the depth distribution of the electrically active boron. By removing this gross damage, without affecting the distribution of the implanted boron, we have determined that the 800°C annealing stage is not exclusively due to the improvement in the crystalline perfection of the amorphous material but also appears to be associated with the annealing of some point defects. These results and their relation to previous results are discussed in the following sections. IMPLANTATIONS Boron ions were implanted into silicon samples using an accelerator capable of operating from 10 to 150

Jan 1, 1970

By Fathi Habashi

METALS COMMONLY leached may come from one of the following sources: 1) Occurring in nature in the native state, e.g., gold, silver, platinum metals, copper. 2) Produced as by-product of a metallurgical process, e.g., gold, silver, platinum metals, selenium. 3) Produced by reduction of an oxide ore, e.g., copper, nickel. GOLD AND SILVER Cyanidation According to Mellor (1923) the alchemists of the eighteenth century knew that gold was soluble in aqueous solution of potassium cyanide, and the early jewelers probably utilized this fact in gilding. He also mentions that Scheele in 1783 and later Bagration in 1843 noted the solvent action of aqueous solutions of alkali cyanides on gold. Yet it was not until 1887 that the value of this observation was recognized, when MacArthur and Forrest (1887) made use of it in leaching gold from its ores. Since then, the process has spread to every gold and silver mining district in the world.

Jan 1, 1970

By T. E. Green

The Bureau of Mines Heavy Metals Program emphasizes the need for improved analytical methods for gold determination. A commercially available ion exchange resin with high selectivity for gold was investigated as a potential method to collect gold from solution. The resin was found to quantitatively collect gold from acid solutions over a wide range of acid concentrations. Common metals were not collected by the resin nor did they seriously interfere with the collection of gold. X-ray spectrographic and neutron activation methods based on the use of papers containing this resin are proposed.

Jan 1, 1970

By W. T. Malone, J. R. Williams, R. L. Tiner, J. M. Tinsley

Hydraulic fracturing methods for production stimulation have become a common procedure in the oil and gas industry. Fracturing treatments are performed on wells of various potentials to help increase the production rate. In addition to the desire for increased production is the need to predict what increase might be expected. This knowledge is useful in economical treatment planning to accomplish the desired production goals for the well. Theoretical production increases due to horizontal radial fractures may be calculated using equations developed from mathematical analyses and electrical models.1,2,6 It also is possible to predict theoretical production increases due to vertical fractures using curves developed from electrical3 and mathematical models.8 However, these studies assumed that the vertical fracture height and the formation height were equal, which may not be true." In addition, the final fracture height through which fluid is produced may not be equal to the created height. The development of vertical fracture proppant transport relationships has made unrealistic the assumption that propped fracture height is equal to created fracture height. Through the use of published proppant transport equations,4'12 it is possible to calculate the height of a bed of propping agent deposited in a fracture of a given height. Assuming that the fluid flowing in the fracture moves through only the propped portion of that fracture (i.e., that the un-propped part of the fracture heals) it becomes essential to know how production increase varies with the ratio of propped fracture height to formation height. It should be recognized that future investigation may determine that the fracture does not heal completely and that a highly permeable channel exists over the deposited bed of proppant. The effect of this channel was not considered for the present study. The following analysis of experimental data allowed development of curves to determine theoretical production increases considering fracture height as a variable. Discussion In designing a fracturing stimulation treatment a number of variables must be considered. The size of the treatment, type of proppant used, proppant concentration, treatment fluid properties and well conditions are all factors affecting the dimensions and permeability of the fracture. Production increase due to a vertical fracture is affected by propped length, height, width and permeability of the fracture for a given set of formation conditions. Production increase may be defined as the ratio of production rate after fracturing to the production rate before fracturing at the same pressure differential, pe — pw. The producing rate in an

Jan 1, 1970

By G. G. Campbell

Bureau of Mines research to develop an in situ retorting recovery method for oil shale has involved field testing of fracturing techniques for creating fluid-flow paths in impermeable oil shale. Electrolinking, hydraulic fracturing without and with sand propping, and explosive fracturing with a liquid explosive were tested in a 25-ft-square, five-spot pattern. These wells were drilled into oil shale at 50-to 88-ft depths near Rock Springs, Wyo. Results of the fracturing tests were evaluated by injecting air into a test well and measuring flow rates and flow profiles in adjacent test wells before and after each test. To identify points of air entry (location of fractures) in wells, flow profiles were determined by use of inflatable packers and by continuous logging with an airflow probe developed during the fracturing program. Electrolinking and hydraulic fracturing without sand propping were relatively ineffective; hydraulic fracturing with sand propping created horizontal fractures with desirable flow capacity; and fracture flow capacity was significantly increased by detonation of nitro-glycerin displaced in the natural and hydraulically induced fracture systems.

Jan 1, 1970

By O. D. Maurice

"This paper will essentially update the information that is already known and published on the limestones of the Province of Quebec. The excellent report by M. F. Goudge (1935)m is difficult to improve upon and the areas of limestone quarrying are generally the same as they were at the time of Goudge's report. Our knowledge of the limestones of Quebec has been improved considerably in recent years by the publications of T. H. Clark, 2 who, since 1938, has been mapping and reporting on these lime-stones and has discussed their stratigraphy, their structural features, their history and their economic value. One economic aspect is the presence of natural gas in these formations and the possible occurrence of oil. A total of 150 test holes had been drilled to a depth of more than 500 feet by the end of 1967 and, in addition, at least 256 more shallow holes had been put down in the St. Lawrence Lowlands. The information from these test holes has greatly improved our knowledge of the thickness and extent. of the various formations of Paleozoic limestone and shale in Quebec.This paper will then review briefly the limestone occurrences in Quebec, using the old as well as the more recent reports as principal references"

Jan 1, 1970

By G. W. Weems

The specific objective of this investigation was to determine the compressibility factors for helium and carbon dioxide mixtures at -10° and -20° C and pressures to 1,000 psia. A Burnett apparatus was used. Data from the experiments were treated by the method of Barieau and Dalton. Tables of compressibility factors and approximations of the virial coefficients are presented for 10 binary mixtures as well as for helium and carbon dioxide. The results follow the same trend as data previously reported.

Jan 1, 1970

By R. L. Christie

"THE ISLANDS lying north of the Canadian mainland, and the large Boothia and Melville peninsulas, form one of the great archipelagos of the world; this sparsely vegetated and nearly unpeopled region extends about 1,500 miles east to west and 1,200 miles from the mainland to the northern tip of the northern-most island. Sea access to most of the islands is restricted by ice to the summer season, and the 'polar pack' ice of the Arctic Ocean presses the year round against the northwest margin of the archipelago. Although the region is remote, the accessibility has greatly increased through a network of weather stations, airfields and air routes connecting with southern centres.The area considered in this paper is that part of the island region underlain mainly by sedimentary rocks. In broad terms, this includes the land and sea areas of the archipelago and the adjacent continental shelf, but excludes the dominantly 'Shield' terrain of Baffin Island, and of Melville and Boothia peninsulas. An impression of the size and potential of this sedimentary region may be gained by comparing some areas: the land area of islands underlain mainly by sedimentary rocks is over 300,000 square miles or about 50,000 square miles greater than the area of Alberta. The total area of the region, including the continental shelf and the inter-island areas, may be double this figure, and may approximate one-seventh of the land area of Canada."

Jan 1, 1970

By W. V. Youdelis, W. H. Bear, G. Cochrane

HERETOFORE, there has been very little study of the effects of various metallurgical factors on the behavior of thermoelectric materials, the need for which is evident if optimum processing and design of thermoelectric devices is to be realized. Accordingly, we have undertaken such an investigation on the thermoelectric materials bismuth and Bi-Sb alloy and in this paper present some preliminary results which merit consideration, in particular the relatively high thermoelectric power and figure of merit values obtained for the Bi-12Sb (at. pct) alloy powder compacts. The thermoelectric parameters for ingot and powder compact specimens are determined and the results are compared with published data for single crystals. Preparation of Materials. The bismuth and antimony used in this investigation are six nines pure. Melting and casting of the ingots was carried out in air for expediency, since most oxidation unavoidably occurs during the preparation of the powder by filing of the ingots. Chill cast ingots of pure bismuth were prepared by pouring the melt into split copper chill molds, and unidirectionally solidified ingots of bismuth and Bi-Sb alloy were obtained by slow directional cooling in pyrex tubes. All melts remained bright during melting and casting, indicating minimum oxidation. Powder for the powder compact samples was obtained by filing the ingots with a fine and coarse file to give a variation in the particle size of the compacts. The particles in the fine powder compacts varied in size from approximately 28 pct less than

Jan 1, 1970

By S. E. Khalafalla

The extremely sluggish oxidation of steel scrap was appreciably accelerated when the charge was pretreated in aqueous solutions of sodium metavanadate or sodium molybdate. The degree of oxidation acceleration was inversely correlated with the melting point of the promoter oxide possessing the highest valency. The magnitude of oxidation enhancement exhibited a systematic inverse dependence on the duration of pickling processes; mere dipping of the oxidizable charge in the vanadate bath was most effective. In general, the rate of steel scrap oxidation increased with increasing concentration of the pickling reagent. The results are explained on the basis of the hydrolytic decomposition of the pickling agent with subsequent slow interaction with the metal surface, coupled with the tendency of vanadium to form polyanions in alkaline media. The data not only served to elucidate the mechanism by which catastrophic oxidation takes place, but also showed that the accelerating species need not be alloyed with the oxidizable metal; surface impregnation by minute amounts of the accelerating species can still produce catastrophic effects.

Jan 1, 1970

By Richard J. Robbins

This paper is presented with particular reference to the findings of the OECD Advisory Conference on tunneling held last July in Washington D. C. A great deal has been said about the Conference in the past few months, but it may be appropriate to review briefly the background and objectives of the Conference to better understand how the mining community can relate its underground excavation problems to the results of the Conference. OBJECTIVES OF THE OECD CONFERENCE The world demand for tunneling (the term tunneling is used here loosely to include almost all forms of underground excavation) is expected to grow at an in- creasing rate. During the decade of the ?70's, the demand is expected to at least double by comparison with the previous decade. Much of this increase in demand will be due to the rapid growth of urbanization around the world. As urban populations grow larger and denser, the conservation of surface land and the quality of the environment become more important. This aspect of the increasing demand poses a difficult challenge to those who must plan and implement urban development.

Jan 1, 1970

By W. F. Chiao

With the application of dislocation damping theory an attempt was made to determine whether the generation and extension of dislocations is inherently more difficult in a brittle steel than in a ductile steel. A ductile steel was compared with a brittle stee1 by simultaneously measuring the ultrasonic attenuation and velocity during tensile test, and the density of free dislocations and their mean loop length were then calculated as a function of strain. The results showed that in the ductile steel there was always a large generation of dislocations and great extension of loop length occurring at some stage within the early plastic region. In contrast, the brittle steel showed very little or no such sudden changes in dislocation dynamic states after the onset of plastic deformation. Furthermore, a strong temperature dependence of dislocation dynamic states was also observed in the ductile steel and a hypothesis was suggested that a thermally activated process of dislocation rearrangement could occur at higher deformation temperatures. The activation energy of dislocation rearrangement at room temperature was estimated as about 2030 cal per mole.C. DUCTILITY is an indispensible property in the application of engineering materials, especially steel. During the past two decades the theoretical and experimental approach to the understanding of flow and fracture of metals has been constantly undergoing changes and progress." while the fracture behavior of metals can be influenced by many factors such as chemical Composition,3 second-phase particle mor-phology,4 and dislocation arrangement,5 it is now a general belief that the fundamental understanding of the ductile-brittle fracture phenomena of solid materials must stem from the study of dislocation dv-namics developed under stress conditions.6,7 Most of the traditional ductility tests, such as Charpy impact test, slow bend test, and tensile fracture test, cannot by themselves reveal directly the mechanisms of ductile to brittle transition of materials. In the experimental investigation of tensile ductility it would be ideal to be able to study directly the dynamics of dis-locations in a bulk specimen during the process of deformation. Since the ultrasonic pulse technique is the only satisfactory method for studying dislocations and the fine details of deformation characteristics in metals in the course of a tensile test, it would appear that a comparative study of ultrasonic attenuation changes during tensile tests of metallic materials exhibiting different ductility might be very informative. So far no work comparable to this study has appeared in the literature. Recent progress in both theory and experiment has indicated the feasibility of studying the dislocation mechanisms of ductility behaviors by ultrasonic measurements during tensile test. Granato and Lucke8 have developed a quantitative theory that enables the calculation of dislocation density and their average loop length from the measurements of ultrasonic attenuation and velocity, and several investigators, including Chiao and Gordon,9'10 have shown that simultaneous ultrasonic measurements can be successfully made during a tensile test. Furthermore, many investigators11-13 have repeatedly proposed in the past several decades that deformation and fracture are mutually self-exclusive, and that the ability or inability of a material to deform plastically, i.e., to generate dislocations, is a major factor in determining whether the material will be ductile or brittle. Thus, in the present work an attempt was made to determine whether the generation and extension of dislocations is inherently more difficult in a brittle steel than in a ductile steel. This article is principally concerned with the study of the relation between the propagation of ultrasonic waves and tensile deformation in a steel series which displays quite different toughness at room tempera-turk. changes in attenuation and velocity of ultrasonic waves have been measured as a function of strain during the deformation process. The results have been interpreted in terms of the vibrating string model for dislocation damping as developed by Granato and Lucke, and it has been found that some of the more subtle predications of the model are in good agreement with the experiments. This would be especially meaningful because most of the previous experiments in testfying the model were carried out with single crystals of high-purity materials and little work has been done with polycrystalline steel alloys. EXPERIMENTAL PROCEDURES AND RESULTS Specimen Materials. The tensile specimens used throughout this experiment were of two compositions selected from a series of Fe-Mo-0.77 pct Mn-0.22 pct C steels prepared for a ductile-brittle fracture transition study. One steel contains 0.21 pct Mo and the other 1.03 pct Mo. These two compositions were chosen for the present study because they possess quite different toughness properties at room temperature. The 0.21 pct Mo steel is quite ductile while the 1.03 pct Mo steel is rather brittle, as measured by the standard Charpy impact test. The alloys had been prepared by vacuum induction melting and chill casting in steel molds. The ingots were hammer-forged into 1/2-in.-sq bars from which tensile specimen blanks were cut. These blanks were first normalized under argon atmosphere at 1700°F and then reaus-tenitized and isothermally transformed at 1050°F to a bainitic microstructure. The chemical compositions, heat treatments, hardness measurements, and Charpy transition temperatures of the two steels are listed in Table I.

Jan 1, 1970

By R. R. Vandervoort, W. L. Barmore

Tensile creep experiments were conducted on high-purity, poly cvystalline rhenium from 1500" to 2300°C at stresses from 1500 to I0,OOO psi in a vacuum of 10-a torr. The apparent activation energy for creep was 60 kcal per mole, and the steady-state creep rate varied directly with stress to the 3.4 power. Dislocation substructure that developed during creep was studied by transmission electron microscopy. Possible rate-controlling deformation mechanisms are discussed. The creep behavior of most metals at elevated temperature can be represented by the following equation:&apos;&apos;&apos; t = Cf(s)(^)(s/E)nD [1] where i = steady-state creep rate, C = constant, f(s) = a function involving microstructure, s = applied stress, E = the average elastic modulus at test temperature, n = constant, D = diffusion coefficient According to this well-established relationship, metals with higher elastic moduli and lower diffusion coefficients should have greater creep resistance at the same stress and temperature and equivalent mi-crostructures. While no diffusion data are available, the diffusivity of rhenium should be less than that for most other refractory metals because of its high melting point and hcp crystal structure. The Sherby-Simnad relation for calculating atomic mobility in metallic systems3 predicts that the diffusion coefficient for rhenium is less than that experimentally determined for tungsten4 in the temperature region 1500. to 2200°C. At these temperatures the elastic modulus for tungsten5 is only slightly larger than the extrapolated modulus for rhenium.6 Thus, rhenium is a good possibility for a a high-temperature structural material, but few data on the creep of rhenium have been reported. This investigation was undertaken to study the high-tempera-ture deformation behavior of rhenium in detail. EXPERIMENTAL TECHNIQUES The material used in this study was consolidated from high-purity powder. After cold pressing the powder to a plate a in. thick, the billet was sintered in hydrogen at 2250°C for 24 hr. The plate was reduced to 0.100 in. by cold cross rolling with intermediate anneals at 1650°C for 20 min between passes. The plate was further reduced to 0.060 in. by unidirectional cold rolling with similar heat treatments between passes, and then finally stress-relieved in hydrogen at 1650°C for 30 min. Specimens tested at 1900°C and below were pretest-annealed at 1900°C for 2 50 hr. Specimens tested above 1900°C were pretest-annealed at 2400°C for 5 hr. The impurity content in the "as-received" plate was quite low, table I. Essentially no change in impurity levels was detected in specimens after creep testing. All creep tests and annealing treatments were conducted in a vacuum of 10-8 torr in a test furnace heated by a tungsten mesh element. The load was applied to the specimens through a bellows, and stresses were maintained to ±1 pct of the selected value by periodic corrections for changes in specimen cross-sectional area during creep and for changes in the bellows spring force due to load column extension. One-inch-diameter tungsten force rods were used in the hot zone of the furnace. Deformation at temperature was measured by optically tracking gage marks on the specimen. Temperature was measured by a calibrated optical pyrometer and was determined to ±5"C. Grain sizes were determined by the linear intercept method and specimens were examined in the "as-polished" condition, using polarized light. Specimens annealed at 1900°C had a grain size of 52 ± 5µ , and those annealed at 2400°C had a grain size of 148 * 11 µ. Pieces were cut from the gage section of creep-tested specimens and planed to a thickness of about 0.010 in. by spark discharge machining. Thin foils for viewing by transmission electron microscopy were obtained by electropolishing in a solution of 6:3:1 ethyl alcohol, perchloric acid, and butoxy ethanol, respectively, using the window technique. Bath temperature was —4OoC, and the cell potential was 35 v. The foils were examined in Siemens Elmiskop I, operating at 100 kv. RESULTS AND DISCUSSION In order to analyze the results from creep experiments, Eq. [I] is rewritten in the following form: <=Kf(s)ne-/RT [2] where K = constant, ?// = apparent activation energy for creep,

Jan 1, 1970

By J. J. Jonas, G. Gagnon

SHG zinc was extruded in the temperature range 110" to 350°C and the strain rate range 0.05 to 5 sec-1 The strain rate/flow stress/temperature results were analyzed using a power sinh stress relationship. When temperature changes due to the heat of deformation and to heat losses are neglected, the exponent of the sinh function of the stress is 5.6, and the apparent activation energy of deformation is 28 kcal per mole. When these changes are taken into account, the exponent decreases to 4.7 and the activation energy to 23 + 2 kcal per mole. The corrected stress exponent and activation energy are in very good agreement with published values obtained from creep experiments, and suggest that the hot extrusion of zinc is controlled by a mechanism involving self-diffusion. When the extrusion and creep data are compared using a Zener-Hollomon parameter and either a sinh or an exponential stress term, an appreciable offset is observed, which may be due to the difference in impurity content. For a given set of extrusion conditions the ram speed, maximum pressure, and initial temperature can also be correlated using a Zener-Hollomon parameter and a sinh pressure term. THE deformation of metals at temperatures over about one-half the absolute melting temperature has been extensively studied at creep strain rates. By contrast, relatively little work has been carried out on the behavior of metals at hot working strain rates. Most of the latter investigations have been performed using simulative methods, such as hot torsion and hot compression, in which the friction conditions and temperature rise during deformation may differ appreciably from those existing under industrial conditions. Recently, however, Wong and Jonas1 used a scaled-down industrial process to determine the stress and temperature dependence of the strain rate during the extrusion of aluminum. In such tests, the effects of friction and adiabatic heating are closer to those produced in industrial operations. Also, with regard to the testing of materials of limited ductility such as zinc, hot compression and hot torsion do not permit the attainment of true strains as large as the deformations usually applied commercially. The present study was undertaken to investigate the extrusion behavior of Special High Grade (SHG) zinc. The detailed objectives were: 1) to establish the stress and temperature dependence of the strain rate with and without a consideration of adiabatic heating, 2) to study the pressure and temperature dependence of the ram speed, and 3) to investigate the microstruc- tural changes occurring during the deformation. The last aspect of the investigation will be covered in a separate paper. The treatment described below differs from that of Wong and Jonas in that the adiabatic temperature rise during deformation is taken into account, and the calculation of the mean equivalent strain rate is based on the redundant as well as on the homogeneous work. EXPERIMENTAL PROCEDURE Rods from two shipments of continuously cast SHG zinc* were used in the investigation. The composition *Supplied by courtesy of Cominco Ltd. range of the impurities present, as given by the supplier, was: Pb: 0.0013 to 0.0023 pct, Fe: 0.001 pct max Cd: 0.0001 to 0.0006 pct, Cu: 0.0002 to 0.0005 pct, Ti: 0.0001 pct max; thus, by balance, zinc valued from 99.9963 to 99.9966 pct. The as-received rods were machined into billets having a nominal diameter of 1.56 in. and a nominal length of 1½ in.; longer billets up to 4 in. in length, were also used to investigate special aspects. The as-machined rods were annealed at 400°C for 24 hr and slowly cooled. This treatment produced a columnar grain structure, with a grain size of about $ by 2½ cm which was appreciably larger than the as-cast one. A 150-ton, direct extrusion, vertical press was used. Ram displacement and force were recorded continuously against time. A constant flow control valve permitted the maintenance of a range of preselected ram speeds up to in. per sec. The selected speed was held constant, irrespective of the required force, as long as the load developed was below the maximum available. Strain gages were used to determine the force; the gages were calibrated before and after each testing period with a 200,000-lb capacity load cell. Further details of the experimental equipment can be found in Ref. 2. The billets were preheated for 90 min in the extrusion container, which was well insulated so as to minimize temperature gradients. This period was sufficient for the billet to reach a uniform temperature at all temperatures between 110" and 350°C. A square-shoulder die having a 0.290-in. diam central hole was used. The extrusion ratio was 30 to 1. This is equivalent to a reduction in area of 96.7 pct, an elongation of 2900 pct, and a true strain of 3.4. The ram speed was varied over two orders of magnitude from 0.0027 to 0.26 in. per sec. The ram was water-cooled during most of the tests, although some experiments were conducted with a preheated, uncooled ram. All extrusions were run without lubricant, which resulted in conditions of sticking friction. EXPERIMENTAL RESULTS Stress Dependence of the Strain Rate Neglecting Adiabatic Heating. The maximum force required to extrude is given in Table 1 for each of the five initial

Jan 1, 1970

By D. P. Pope, T. Vreeland

Observations of dislocations in zinc using Berg-Barrett X-ray micrography confirm the validity of a dislocation etch for (1010) surfaces. A technique for measurement of the depth in which dislocations can be imaged in X-ray micrographs is given. This depth on (0001) surfaces of zinc was found to be 2.5 µ using a (1013) reflection and CoKa radiation. BUCHANAN and Reed-Hill (B & RH) have recently questioned the ability of a dislocation etch to reveal all of the basal dislocations which intersect (1010) surfaces in annealed zinc crystals.&apos; This etch was developed by Brandt, Adams, and Vreeland who conducted a number of different experiments to check its ability to reveal dislocations.2,3 B & RH prepared (0001) foil specimens for transmission electron microscopy from annealed crystals and observed dislocation densities of about l08 cm per cu cm in the foils, while the etch indicated densities of the order of l04 cm per cu cm in their annealed crystals. As this etch has been used in a number of studies of dislocations in zinc, it is of considerable importance to reassess its validity in the light of the B & RH results. The X-ray work reported here was undertaken to check the ability of the etch to reveal dislocation intersections on (1070) surfaces of zinc. The X-ray technique was chosen for this check because it could be applied to the as-grown crystals with a relatively small amount of specimen preparation. We believe that the possibility of accidental deformation in preparation of the bulk specimens is considerably less than that for thin foil specimens suitable for transmission electron microscopy. Unfortunately, basal dislocations are not visible on Berg-Barrett topo-graphs of (1010) surfaces, which are the surfaces on which the etch is most effective. Therefore, a one-to-one correspondence between the etch and X-ray observations could not be made. Basal dislocations near (0001) surfaces have been observed by Schultz and Armstrong4 using the Berg-Barrett technique, but they did not report the as-grown dislocation density observed in their crystals. We have applied the X-ray technique in this study to surfaces oriented from 1 to 2 deg of the (0001) to determine the basal dislocation density, and have compared this density with that observed using the etch on a (1070) plane of the same crystal. The X-ray observations permit determination of the depth in which basal dislocations can be observed under the diffracting conditions used. SPECIMEN PREPARATION High purity zinc crystals are very soft, so a good deal of care must be exercised in the preparation of observation surfaces. As-grown crystals approximately 2.5 cm in diam and 20 cm long were acid cut into 1.25 cm cubes. A thin slab was cleaved from an (0001) surface to produce an accurately oriented reference surface on the specimen. Some of the cubes were examined in the as-machined condition while some were annealed in argon at 410°C for 2 hr. Heating and cooling rates were less than 2°C per min. Some of the specimens were scratched on a (0001) surface with a razor blade to produce fresh dislocations. Approximately 2 mm of material was acid lapped from one face of a cube to produce a surface oriented between 1 and 2 deg from the basal plane and parallel to the [1210] direction. A (1070) surface was also acid lapped. The lap used a 1 to 3 pct solution of HN03 in water to saturate a soft cloth which was backed by a stainless steel plate. The cloth was moved over the crystal surface at a rate of 20 cm per sec while a normal force of about 4 g was maintained between the cloth and the specimen. As-lapped surfaces were examined as were surfaces which were chemically and electrolytically polished after lapping. The small angle between a lapped surface and the (0001) plane was measured to 0.1 deg using a Unitron microgoniometer microscope (the cleaved surface was used as a reference in this measurement). The microscope was modified so that the intensity of reflected light could be continuously monitored on a meter. This modification produced nearly a ten-fold increase in the reproduceability of orientation readings. OBSERVATIONS The Unitron Microgoniometer observations indicated that the lapped surfaces had a terraced structure with the terraces quite rounded and spaced about 0.1 mm in the [1010] direction. The maximum change in slope between terraces was 0.25 deg, indicating a terrace height of about 0.1 µ. A Unitron measurement of the average angle between (0001) and a lapped surface was checked by micrometer measurement of the specimen and found to agree within 0.1 deg. The Berg-Barrett micrographs using (1013) reflections and CoKa radiation5 revealed subboundaries, short dislocation segments, spirals, and loops near the surfaces which were oriented from 1 to 2 deg of the (0001). Micrographs of surfaces prepared by lapping appeared very similar to those of the chemically and electrolytically polished surfaces. The loops and spirals were not extinct in (1013) or (0002) reflections, indicating that they have a nonbasal Burgers vector. Extinctions of the short, straight dislocations indicated that they belonged to an (0001)(1210) system. Fig. 1 is an example of a micrograph which shows a subboundary, and dislocation segments which are pre-

Jan 1, 1970

By P. A. Richardson

The current Bureau of Mines active list of permissible explosives includes 76 brands. Eleven are gelatinous and the rest are the granular type. The list of permissible blasting devices comprises five Cardox models.

Jan 1, 1970

By F. P. Haver

A procedure is described for recovering both lead and sulfur from galena flotation concentrate, comprising the following steps: (1) Aqueous oxidation of the concentrate, using ferric sulfate to convert lead sulfide to sulfate and to give elemental sulfur; (2) regeneration of the ferric sulfate by electrolysis in a diaphragm cell; (3) treatment of the leach residue with ammonium carbonate solution to change the lead to an acid-soluble form and to produce ammonium sulfate as a byproduct; (4) solution of the lead carbonate in hydro-fluosilicic acid followed by electrolysis to recover the lead as metal and regenerate the acid; and (5) extraction of the elemental sulfur from the final residue with an organic solvent. About 90 percent of the lead can be recovered by the above method as 99.9-percent-pure metal, together with two-thirds of the sulfur--half in the elemental form and half as ammonium sulfate.

Jan 1, 1970

By R. G. Aspden, D. A. Colling

THE {120}(001) texture has been reported in near 50 pct Ni-Fe alloys <0.004 in. thick1,2 and in copper 0.014 in. thick.3 This texture is one of two types of secondary recrystallization textures observed to replace a cube texture matrix and is desirable in Fe-Ni alloys because of its unique magnetic characteristics.1,2 However, the conditions for and mechanism of the {120}(001) formation are not well understood.3 During an investigation of the influence of alloying elements on the magnetic characteristics of 49 pct Ni-Fe alloys with a sheet thickness of 0.014 in., we have observed the growth of {120}(001) secondaries when strong deoxidizers such as aluminum and calcium were present. It is believed that this observation in unique and provides additional insight with regard to the mechanism for {120}(001) texture formation. Three alloys were prepared with electrolytic iron and nickel and contained a nominal 49 wt pct Ni. Alloy A was a straight binary Fe-Ni alloy, whereas intentional additions of 0.013 wt pct Ca to alloy B and of 0.59 wt pct A1 to alloy C were made. Ingots were forged at 1100 C, hot-rolled to 0.150 in. gage, pickled, and cold-rolled to 0.014 in. Standard U-shaped magnetic test specimens were punched, deburred, sprayed with MgO, and annealed in ~50°C dew point hydrogen. Textures were identified with the aid of etch pits, the

Jan 1, 1970

By W. C. Hellyer

In an autogenous grinding circuit in which feed at approximately nine inches top size is reduced to a size suitable for subsequent processing, the build- up of a "critical size" fraction in the media causes problems. A "critical size" fraction has been defined as, "media too small to effect reduction by impact grinding of ore coarser than a quarter of an inch and too large to be broken by the largest size of media in the charge. 9, (1) The buildup of a "critical size" fraction reduces the capacity of the mill, increases the grinding power requirements per ton of finished product, and generally produces a finer grind than is desired. It is general practice to overcome this problem by the addition of large diameter steel balls to the grinding charge. This has certain disadvantages, such as; (i) an increase in mill liner wear; (ii) wear on the steel balls, and; (iii) some loss in flexibility in grinding circuit operations resulting from difficulties in removing the steel balls by means other than by grinding out.

Jan 1, 1970