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By C. C. Koch, M. L. Picklesimer

PHYSICAL metallurgists interested in the alloying behavior and phase transformations in rare-earth metals and alloys require a strain-free polished and etched surface for both metallographic and X-ray examination. However, the rare earths have presented a problem in this respect since they are difficult to polish free from strain and are very reactive to the atmosphere. Their tendency to oxidize readily even at room temperature necessitates careful preparation and rather elaborate protection if their surface is to be examined for any length of time. The "light" lan-thanides (i .e., atomic numbers less than 63), especially lanthanum and cerium, are particularly bad in this regard; they oxidize very rapidly at room temperature. To eliminate the problem of plastic deformation remaining on the surface after mechanical polishing, electropolishingl and chemical polishing techniques2 have been developed. The electropolishing technique requires the specimen to be immersed in an electrolyte at -77°C and thus obviates a metallographic study of, for example, the fcc —double-hexagonal close-packed (dhcp) transformation in cerium which begins at -10°C. The chemical polishing solution has been used only on several of the "heavy" rare-earth metals. However, a convenient method for protecting the polished and etched surfaces from atmospheric corrosion has not been available. Our interest in the superconducting properties of lanthanum, and in the phase transformations in lanthanum and cerium, has led us to develop a technique for the metallographic preparation of lanthanum and cerium which clearly reveals the microstructure and preserves the etched surface for days. The specimens are chemically polished and anodized. The chemical polishing is performed at room temperature, the anodic oxide film provides the required protection from the atmosphere, and colors produced in the film provide a simple positive technique for phase identification. Lanthanum and cerium metal ingots obtained from Johnson Matthey and Co., Ltd., were remelted to suitable shapes and heat-treated to produce various microstructures. The samples were placed in epoxy mounts and, after a small hole was drilled in the back of the mount for electrical contact, were ground on silicon carbide

Jan 1, 1968

By J. Tarwater

The torsional testing of cylindrical medium-carbon steel specimens, heat treated to a high strength level, revealed a stress-strain relationship that was dependent on the direction of torsional plastic pre-strain. This Bauschinger effect was observed in prestrained specimens both with and without subsequent elevated-temperature strain aging. Yield stresses in strain-aged specimens exceeded those of simply prestrained specimens and the difference in stress was greater when the prestrain direction opposed the test direction. This behavior is discussed in terms of the classical dislocation pile-up using Cottrell's equation, A plastically prestrained strain-hardenable member, loaded in a direction opposite to the direction of prestrain, produces a stress-strain relationship differing appreciably from the curve representing reloading in the prestrain direction. This phenomenon, referred to as the Bauschinger effect, will be discussed in terms of the stress differences ob- served at a specified strain. The effect, dating back to the 1880's, was first attributed to grain boundary stresses. When later work revealed that the effect was also present in single crystals, revised theories attributed the diminished applied reverse stress to assistance from internal long-range stresses. These stresses have been associated with dislocation pile-ups or with dislocation arrays having analogous stress patterns. The stress patterns are subject to alteration by interaction with interstitial solute atoms and acceleration of the interaction may be accomplished with elevated-temperature strain aging. As discussed herein, the interaction showed a directional effect with regard to the applied stresses necessary for small plastic strains. Aside from the rigorous Bauschinger stress-strai relationship, which compares prestrained members, it is interesting to compare the stress-strain curve of a member being prestrained with that of a prestrained member being reverse loaded. For small strains which are a fraction of the prestrain deformation, the applied stresses of the reverse reloaded member are smaller. However, as the reverse strain approaches the prestrain value, the stresses approach equivalence. It has been reported1 that the stress required to return a prestrained specimen to its initial "zero" position generally exceeds the prestrain stress because of the work hardening occurring on potential slip systems during prestrain.

Jan 1, 1963

By J. C. Uy, A. A. Burr

A quantitative relationship between the allotropic phase boundaries of zirconium-base binary systenzs and the solute metallic valence is shown through an intermediate thermodynamic parameter. A simplified equation relating this parameter to the phase boundaries is briefly reviewed, and data from the literature are used to show the relationship of this parameter to the solute metallic valence. It has been reported that the solute metallic valence can be used as an index of phase stabilization in zirconium-base binary alloys.' It was shown that the algebraic sign of the slopes of the hcp/bcc phase boundaries of zirconium alloys correspond to the algebraic sign of the metallic valence of zirconium minus the metallic valence of the solute, or, in other words, a solute whose metallic valence is higher than that of the solvent tends to stabilize the high-temperature phase while one whose metallic valence is lower than that of the solvent tends to stabilize the low-temperature phase. Further analysis of the zirconium binary systems has revealed a quantitative relationship between the solute metallic valence and the relative slopes of the two-phase allotropic boundaries. This relationship involves a thermodynamic quantity whose significance can be seen in the following section. PHASE-STABILIZATION PARAMETER Let Qb be the difference between the partial molar heats of mixing of a given solute in the two allotropic phases of the solvent which are in equilibrium with each other at a given temperature, thus A relationship between this term Qb and allotropic phase boundaries has been employed by several au-thors'-= in the evaluation of phase diagrams, and can be briefly derived as follows. Referring to Fig. 1, consider the general case of two allotropic phases, each having a small mole fraction (Xa,Xb) of the solute, in equilibrium at temperature T and atmospheric pressure as represented by the reaction. solute in ß phase =solute in a phase If now a reaction occurs such that an infinitesimal amount of the solute is removed from the ß phase and added to the a phase, there would be a partial molar

Jan 1, 1967

By C. W. Hill

FLUXES, in general, may be classified according to their use as soldering, foundry or casting, and metallurgical and the chemistry of their action follows quite closely this division. The term foundry or casting fluxes, as used here, refers to the substances added to molten metals, preparatory to casting into molds or ingots, with the object of removing small amounts of impurities that have been introduced in handling or melting the metal, which was placed in a fair state of purity by the previous refining or metallurgical processes. The sources of these impurities are the oxide coating on the surface of the ingots, material extracted or mechanically removed from the crucible or furnace wall, and those formed by the reaction of the molten metal with the heating gases or furnace atmosphere. As commonly used, the term fluxes is applied to such materials as ammonium chloride, zinc chloride, salt, borax, and boric oxide. A second class of materials, usually called deoxidizers, includes substances, such as metallic phosphides, sub-oxides, carbides, and bo-rides, that reduce the metallic oxides present in the metal. A third class includes various compounds that are molten and non-volatile at the temperature of the molten metal and are used primarily to protect the surface of the metal from the action of the furnace or exterior atmosphere; to this class belong such mixtures as lime and fluorspar, lime and soda ash, various minerals, etc. In some cases these protective layers may act in a manner similar to the metallurgical fluxes and dissolve or unite with the oxide impurities of the metal, but as generally employed this latter action is negligible since there is little opportunity for the coverings to come into contact with more than the surface of the metal, and hence they are without action on the body of the molten mass. The use of fluxes is the result of factory experience and tradition, but an extensive study has not been made of the chemical, and physical actions that occur or the effects of these actions on the properties of the metal. It would seem necessary in any successful study of metal fluxes

Jan 10, 1920

By E. S. Bardwell, R. J. Lapee

Twenty years ago, W. T. Burns, in his paper presented at the Butte Meeting of the Institute,' discussed the general scheme then in use in the electrolytic copper refinery of the Anaconda Copper Mining Co. at Great Falls, Mont., for removing impurities from tank-room electrolyte and controlling its acid content. Since then marked changes have taken place in copper-refinery practice at Great Falls. The electrolytic copper refinery in use in 1913 has been replaced by a new and entirely modern plant capable of producing up to 27,000,000 Ib. of cathode copper per month. With the building of the new plant in 1916, the treatment of converter anodes was discontinued. At first the substitution of refined anodes for converter anodes resulted in a decrease in the impurity content of the anodes, but as time went on, changes in metallurgical practices at the smelter resulted in substantial increases in the impurity content of the anodes. The leaching of the silver slime to remove copper before shipment to Raritan for treatment further added to the purification problem. The fact that the scheme of purifying electrolyte which Mr. Burns described in his paper has proved adequate for our needs under a wide variation of conditions speaks well for its essential soundness. Method of Purification Briefly, the method adopted for purifying tank-room electrolyte at Great Falls has been as follows: Each day a certain volume of tank-room electrolyte is run off and sent to the purification plant, where it is boiled down to approximately 46' 136. The concentrated electrolyte is then sent to crystallizing tanks where the bulk of the copper is crystallized out as copper sulfate. The mother liquor is then passed through insoluble anode tanks to remove the last of the copper and most of the arsenic and antimony. It is then either returned to the tank room direct or boiled down to 55' Bé, the iron and nickel salts crystallized out and the mother liquor returned to the tank-room circuit as restored acid. Prior to 1930 all of the evaporating was done in lead-lined tanks 13 ft. in diameter by 4.5 ft. deep, provided with lead heating coils through which steam at 30 lb. gage pressure was circulated.

Jan 1, 1934

By W. B. Vietz, C. W. Hill, T. P. Thomas

FLUXES, in general, may be classified according to their use as soldering, foundry or casting, and metallurgical and the chemistry of their action follows quite closely this division. The term foundry or casting fluxes, as used here, refers to the substances added to molten metals, preparatory to casting into molds or ingots, with the object of removing small amounts of impurities that have been introduced in handling or melting the metal, which was placed in a fair state of purity by the previous refining or metallurgical processes. The sources of these impurities are the oxide coating on the surface of the ingots, material extracted or mechanically removed from the crucible or furnace wall, and those formed by the reaction of the molten metal with the heating gases or furnace atmosphere. As commonly used, the term fluxes is applied to such materials as ammonium chloride, zinc chloride, salt, borax, and boric oxide. A second class of materials, usually called deoxidizers, includes substances such as metallic phosphides, sub-oxides, carbides, and bo-rides, that reduce the metallic oxides present in the metal. A third class includes various compounds that arc molten and non-volatile at the temperature of the molten metal and are used primarily to protect the surface of the metal from the action of the furnace or exterior atmosphere; to this class belong such mixtures as lime and fluorspar, lime and soda ash, various minerals, etc. In some cases these protective layers may act in a manner similar to the metallurgical fluxes and dissolve or unite with the oxide impurities of the metal, but as generally employed this latter action is negligible since there is little opportunity for the coverings to come into contact with more than the surface of the metal, and hence they arc without action on the body of the molten mass. The use of fluxes is the result of factory experience and tradition, but an extensive study has not been made of the chemical and physical actions that occur or the effects of these actions on the properties of the metal. It would seem necessary in any successful study of metal fluxes to determine not only what impurities are present in metals melted under

Jan 1, 1921

By P. D. I. Honeyman

Changing trends in concentration, involving regrinding with the subsequent production of a finely divided, high-grade flotation product, presents a real problem to the modern copper smelter. In the treatment of such a material, handling difficulties are numerous and potential possible losses may be very great. In many plants, of course, preliminary roasting of the furnace charge remains an economical necessity. Under such circumstances, the operator has no alternative except to follow orthodox roaster reverberatory practice, though taking all possible precautions to avoid excessive dust losses and bad working conditions. In other plants, roasting is not only unnecessary but would be highly undesirable, and at best the charge would be merely dried before entering the reverberatory furnace. In the latter case the possibilities of raw charging loom large. The Miami plant of the International Smelting Co. handles the entire output of concentrates of the several mining companies operating in the Globe-Miami district. All of these companies produce a flotation concentrate which, at the Miami Copper Co. particularly, is all reground and is high in grade. In addition, the Inspiration Copper Co. ships a substantial tonnage of high-grade cement copper to the smelter from its leaching plant. Following the flow sheet of the original plant, all such material received was bedded, dried in Wedge furnaces and smelted in reverberatory furnaces. At times during the history of the plant it has been necessary to carry the drying operation further, to a partial roast, before reverberatory smelting. Since the charge contained over 80 per cent flotation concentrates, the handling of which in a dried condition was at best a dusty job, unusual precautions were taken to cut down dust losses. The Wedge furnace plant was equipped with a Cottrell treater and all hoppers and calcine cars were carefully designed to cut down dust loss in transferring the so-called calcine from hoppers to car and from car to furnace. In the furnace itself the dusting problem was a severe one. Arch erosion was very rapid and flues and waste-heat boilers rapidly filled up with a partly smelted flue dust.

Jan 1, 1934

By R. L. Skaggs, R. A. Molsberger

DARKEN1 has pointed out that in most binary liquid metal systems the thermodynamic behavior is relatively simple in the terminal regions. Between the terminal regions. the thermodynamic behavior is more complex. To describe this behavior. he has defined the stability and the excess stability as shown: Qualitatively, an inflection in the free energy of mixing curve results in a change in sign, from positive to negative, of the stability function and is associated with a phase separation. Conversely, a large, positive stability over a narrow composition range is indicative of compound formation. Darken has shown a number of binary systems where the excess stability is constant in the terminal regions and varies sharply in between. The work described in this communication was undertaken to study the variation of stability and excess stability in a binary system as a function of temperature. In addition, this work provides means for the direct comparison of previously existing equilibrium (activity) and calorimetric (molar heat of mixing) data on the Hg-Sn system. Hildebrand2 measured the vapor pressure of mercury over Hg-Sn alloys at 595°K. Calorimetric studies were made by Kawakami3 at 523°K and by Kleppa4 at 423°K. In this work, the equilibrium vapor pressure of mercury was measured over a series of Hg-Sn alloys at 453" and 503°K by use of fused salt manometer with one arm exposed to mercury vapor. Deflections of the fused salt manometer were balanced by argon pressure on the other arm. Argon pressure was subsequently measured with a dibutyl phthalate manometer. Tin activities were determined by graphical integration of the Gibbs-Duhem equation making use of the familiar Darken5 a function. The activities of mercury and tin showed positive deviation from Raoult's law at 453 and 503°K as Hildebrand observed at 595 K. In Fig. 1 are plotted log activity of mercury and tin vs reciprocal temperature. The plot contains activities obtained from calorimetric studies. Hult-gren6 has calculated activities from Kleppa's4 data, and Kubaschewski7 has similarly treated Kawakami's7 data. Presumably. in each case a regular solution was assumed. For regions where a two-phase field

Jan 1, 1970

By Cleland N. Conwell

Intermittent coal mining has been conducted in Alaska for over a century. The first report of coal in Alaska was by the Veechy expedition of 1826 and 1827. Whaling ships used coal from Corwin Bluff near Cape Beaufort during the early and latter parts of the 19th century. The first coal mine in Alaska-and probably the oldest in the Pacific coast of North America-was opened by the Russians at Port Graham on the southwest tip of the Kenai Peninsula. The mine was operated from 1855 until 1867 when the United States took possession of Alaska. From 1880 to 1915 coal mining was carried on intermittently at several localities including Unga Island, Herendeen Bay, Chignik Bay, Kachemak Bay, and several points along the Yukon River. Small coal mines along the Yukon River provided fuel for the river steamers traveling from St. Michaels to Whitehorse. The area of sustained coal production began with the completion of the Alaskan Railroad from Anchorage to the Matanuska coal field in 1916 and to the Nenana field in 1918. Coal production continued to increase until 1953, at which time the oil and gas fields in Cook Inlet were developed. Oil and gas eventually replaced the Matanuska coal as a means of providing heat and power. The military in the Anchorage area shifted from coal to oil in 1967 causing a decrease in production. The increased demand for electric power in the Fairbanks area offset the decline and coal production started to increase. In 1969-1970 the Golden Valley Electric Assn. (GVEA) constructed a mine-mouth power plant 70 miles southwest of Fairbanks near Healy and a power line to Fairbanks. Location of Coals in Alaska Coals are found in all geographical subdivisions of Alaska. Coal in Alaska ranges in age from Carboniferous to Tertiary, and grade from lignite through anthracite. Fig. 1 shows the locations of Alaskan coal fields. The only fields that have been developed extensively are the Matanuska and Nenana. Fig. 2 illustrates the annual production of coal in Alaska and the ratio of underground to strip mining.

Jan 1, 1973

By J. J. Quinn

Several mineral flotation plants utilize process water with high soluble salt content. The processing of semi-soluble minerals, the use of recycle streams, sea or well water give rise to this situation. It is unclear as to the overall effect on flotation response though there does seem to be evidence of bubble size reduction, increased froth stability and reduced reagent dosage. The present work aims to quantify the effects of salts present in process water on gas dispersion (bubble size and gas holdup) and froth properties. The salts examined were NaCI, CaCl2, Na2SO4, Na2S2O3 and Al2(SO4)3. Tests were conducted to determine the effects of salt type and concentration on gas holdup and bubble size distribution. The salts containing multivalent ions had a greater impact than the monovalent ions, in keeping with the literature. A relationship between gas holdup and ionic strength was established. The concentration of frother (methyl isobutyl carbinol, MIBC) giving equivalent gas holdup was determined. The effect of salt and frother combinations was also explored.Proposed mechanisms for coalescence inhibition in salt solutions are briefly reviewed in light of the current findings.

Jan 1, 2006

By T. F. Archbold, P. G. McCormick

Silica fiber 11arkevs and hardness irzdentatiozs have been used to study the thermal diffusion of racancies in zinc placed in temperature gradients of 460o and 706oK per Cm All markers mored toward the higher temperatures, and the data show that the heat of trarlsport Q is greater than the eizthalpy of z,acancj3 forrjalion E by an amount equal to 3.5 kcal per mole. These results ore not in agreement with those obtained in either of the two previous studies with zinc. The problem is discussed in terms of experimental differences and racancy source and sink efficiencies. THE general interest in thermal-diffusion phenomena over the past several years has prompted a number of marker movement studies using pure metals. In order to understand better the relationships between thermal and mass flow, a general goal of the experiments has been to obtain values for the net enthalpies carried by the diffusing atoms. For self-diffusion by means of the vacancy mechanism, the determination of relative marker positions before and after an anneal in a temperature gradient permits a calculation of a value for (Q - Ef). Q is the transferred enthalpy, and Ef is the enthalpy of vacancy formation in the metal being investigated. The initial experimental study of thermal diffusion in pure metals was accomplished by Shewmon who found essentially no movement of surface-hardness indentation markers in single and bicrystals of zinc held for 20 days in a temperature gradient of 310°C per

Jan 1, 1967

By L. Gunnewiek

An advanced real-time monitoring system called the tapblock diagnostic system (TDS) has been developed. The purpose of the TDS is to help furnace operators manage the safe operation and economical maintenance of furnace tapblocks. This system is an evolution of the current practice of using historical records and operator interpretation to assess the ?health? of a tapblock. The main parameters affecting tapblock health are heat removal capacity and refractory wear, and these are currently difficult to assess in situ except in a global way. By using monitored and operating data together with predictive numerical modelling and multivariate statistical methods, real-time tapblock performance is assessed relative to expected performance. A state indicator in the form of a green, yellow, and red light is used by furnace operators to monitor the tapblock performance and health status during operation. Access to historical operating data and the provision of diagnostic functions allow for probable health degradation events to be deeply investigated. A recent opportunity to evaluate the actual performance of a first generation TDS installed in the KIVCET furnace at Teck Cominco?s Trail Operations showed that a reasonable estimate of tapblock health was made. However, the evaluation also found that some areas of refractory wear were missed, and a new mechanism affecting refractory wear was discovered that was not previously known. This has reinforced the belief that there is a need to develop improved methods of monitoring so that data used to define the health of the tapblock is more comprehensive and accurate.

Jan 1, 2008

The Australian Coal Combustion Testing and Research Facility has been operating commercially for one year and during that period coal product evaluations have been conducted on behalf of four coal companies and one electricity commission. The facility is equipped to assess the behaviour of steaming coal in milling, combustion (including flame stability, burnout and heat transfer), ash deposition and erosion, fly ash collection and gaseous emissions. The relevance of the results of the pilot testing to industrial practice was demonstrated during the calibration of the facility using four coals burnt in Australian power stations. The calibration coals were from the Tarong and Gladstone Power Stations in Queensland, tluja Power Station in Western Australia and Bayswater Power Station in New South Wales. Also an opportunity arose to visit an overseas power station to observe a full scale test burn using one of the early coals tested on a commercial basis in the combustion test facility. The calibration trials showed excellent agreement with industrial coal performance in t:orms of flame stability, turndown, carbon burnout and gaseous emissions. Encouraging correlations were also found in the case of furnace radiation, boiler deposits (slagging and fouling) and electrostatic precipitation. In the case of the last group the only real reservations about the correlations are due to the non-availability or qualitative nature of results collected around the power stations. In all cases there is a high degree of confidence in the facility's ability to predict the relative performance of different coals and in some cases direct numerical predictions can be Made.

Jan 1, 1987

By F. R. Hensel

Up to the present time few attempts have been made to produce hard nonmagnetic materials by heat treatment of austenitic steels. The usual result has been to cause them to pass into the martensitic stage, thus destroying to a great extent the typical austenitic properties, since this involves a transition of a portion of the iron from a face-centered to a body-centered type of atomic arrangement. High-strength nonmagnetic materials such as might be provided by properly hardening austenite are required in the electrical industry for different machine parts. In Europe nonmagnetic retainer rings for restraining the end-turns of the rotor windings in turbo-alternators have been developed as a special application of high-strength austenite. In testing1 a 28,000-kva. three-phase Siemens turbogenerator running at 3000 r.p.m. at full load current, the losses in the short-circuit test were 450 kw. for the magnetic ring and 286 kw. for the nonmagnetic, and the difference should be attributable to the magnetic ring. The differences in temperatures during the same test are given in Table 1 and these show the advantage of a nonmagnetic over a magnetic retainer ring. Hardening in this case was obtained by cold working, such as hammering, rolling or some means for stretching the steel while at a temperature near 500" C. One means for stretching2 is to rotate the forged or rolled ring in a centrifugal machine so as to develop within it stress higher than

Jan 1, 1931

By H. J. Engell, W. Frank, A. Seeger

SWISHER and ~urkdogan' have determined the solubility of oxygen in a iron. They found it to lie between 7 and 10.5 at.-ppm at 881°C. Using earlier work on the permeability of oxygen in bcc iron,' they arrived at the following expression for the diffusion coefficient of oxygen in bcc iron (k = Boltzmann's constant, T = absolute temperature): where The present authors3 have estimated the activation energy QD for the diffusion of oxygen in bcc iron in two different ways from various experimental data.2'4"6 In the first method QD + QS (QS = heat of solution for oxygen in bcc iron in thermodynamic equilibrium with solid FeO) was determined either from data on the reduction of FeO with hydrogen4 or from measurements of the internal oxidation of silicon in a iron.5 Using an estimate of QS from investigations of the oxygen solubility in 6 iron2 (in thermodynamic equilibrium with molten FeO) Q = 0.97 ev or Q~ = 1.06 ev were obtained. From the magnitude of these values it was concluded that oxygen migrates interstitially in bcc iron and that consequently the activation energy QD for diffusion of oxygen has to be identified with the migration energy E~ of the oxygen atoms. Therefore, for a second estimate of QD from the diffusion coefficient of oxygen in 6 iron at 1450" ~,~ we used the theoretical expression:3 (a = length of elementary cube edge, m = mass of interstitially diffusing atom, sM = migration entropy), applicable to diffusion via the octahedral interstices in bcc lattices. Taking sM = 3.8 k (migration entropy of carbon in a iron), one gets Q = 0.90 ev. Hence, in Ref. 3 Q = (0.98 *0.1) ev was proposed as a plausible value for the diffusion energy of oxygen in bcc iron. sM + 9 (9 = solution entropy for oxygen in bcc iron) can be determined from permeability measurements.4 Using the above-mentioned estimate for QS , the following expression for the solubility c (atomic concentration) of oxygen (in thermodynamic equilibrium with solid FeO) in bcc iron was derived: From [4] the solubility of oxygen at 881°C in a iron is calculated to lie between 0.6 and 12 at.-ppm. We see that the solubility determined by Swisher and

Jan 1, 1969

By J. E. Lawver, G. L. Samsel

The success of many mineral dressing processes, including froth flotation and electrical concentration, depends largely on knowledge of physical and chemical structures of the mineral surfaces involved. As a general rule solids have surface layers, usually invisible by optical tests, that differ from the substratum. To the mineral engineer, therefore, a knowledge of the surface structures of minerals is of paramount importance. During the past decade one of the most powerful tools in the study of froth flotation mechanisms has been the use of radioactive tracers, but this technique usually cannot give definite information regarding the chemical changes that may or may not have occurred at the surface. The electron microscope and electron diffraction camera can be particularly useful instruments in surface studies.. An election microscope permits much closer examination of surfaces than can be obtained with a petrographic microscope. In certain cases, it is possible to identify trace quantities formed by chemical reaction between flotation agents and mineral surfaces by the use of a single-crystal, reflection electron diffraction camera. This article describes several instances in which these instruments have been valuable guides in mineral dressing research at International Minerals & Chemical Corp. One of the first applications of these techniques employed by International Minerals was in conjunction with the study of electrical concentration of potash ore. The first reasonably successful separation of potash ore was made by subjecting a sample of the ore to a methanol wash. Subsequent tests using tagged 6C14 methanol showed that only a minute quantity of radioactivity was detectable after the methanol-washed sample had been dried and heated to about 300°F. It was concluded that although some methanol had been held to the surface by adsorption, this could not account for the improved electrification because there was no evidence of methanol selectivity with respect to NaCl or KCl. Consequently there must have been some other change in the surface. Carbon replicas* of the mineral grains were made before and after the methanol wash. The replicas were separated from the minerals by dissolving in water. This extraction replica technique is particularly attractive because the specimen can first be used with the electron microscope to observe the general structure of the surface and can be re-used as a specimen for electron-diffraction studies to identify any solvent insoluble material present on the mineral surface." Fig. 1 shows the general

Jan 1, 1960

By Y. C. Liu, W. R. Hibbard

An aluminum single crystal cold-rolled from (110) [1121 essentially retains its initial orientation after 99.6 pct reduction in thickness. The orientation of the recrys-tallized grains of this material can be described in terms of crystallographic rotations about principal poles of deformation texture. DURING the study of the recrystallization of a copper single crystal cold-rolled from a (110) [112] initial orientation, the orientation of the re-crystallized grains could be derived by a 30" rotation of the orientation of the cold-rolled matrix about its <111> poles.&apos; The present investigation was undertaken to extend the work done on copper&apos; to an aluminum crystal also cold-rolled from a (110) [112] initial orientation. Experimental Procedure The procedure of this experiment was similar to that reported for copper.&apos; An aluminum (99.998 pct) single crystal rod* 1 % in. in diameter was grown in back-reflection technique.&apos; The specimen (1.20x 1.004x0.6787 in. thick) was then rolled along the [112] direction. The final thickness was 0.0028 in., giving a reduction in thickness of about 99.6 pet. Specimens were cut from the rolled strip with scissors, and approximately in. of disturbed metal was removed with Tucker&apos;s reagent. The rolling edge remained intact. The specimens were sandwiched between two graphite plates and annealed in a lead or lead alloy bath which was electrically heated. Pole figures were constructed using the techniques previously described.&apos; Specimens were electrolytically polished4 and etched with 47 pct HNO8, 50 pct HC1, and 3 pct of 48 pct HF. The electrolytic polishing method and etching reagent employed for aluminum specimens were not entirely satisfactory and the microstruc-tures could not be studied in any detail. Results and Discussion The octahedral pole figure of cold-rolled aluminum strip is plotted in Fig. 1. The <111> poles spread in the transverse direction approximately 8" for the highest intensity areas. The spread in the transverse direction can be related to a rotation about two <110> directions lying in a plane containing the rolling direction and rolling plane normal. The two <110> directions and a scale of rotation for the <111> poles are shown in Fig. 2. The amount of rotation is consistent for three of the four <111> poles, about 35" to 40". The discrepancy for the fourth pole is believed to be due to limitations of the film technique. Alternate inter-

Jan 1, 1956

By O. D. Sherby, J. E. Dorn, C. D. Wiseman

MCLEAN&apos; has shown that the total strain obtained during creep of aluminum polycrystals arises exclusively from the mechanisms of 1) microscopically observable slip, 2) subgrain tilting, and 3) grain boundary shearing. Extensive analyses, however, suggest that the high temperature creep of metal polycrystals is controlled by a single thermal activation process."" These somewhat contradictory observations might be reconciled if it could be shown that the activation energies are identical for each of the mechanisms isolated by McLean. Such identity of the activation energies, of course, would demand that the same unit process controls the functioning of each individual mechanism. Under these conditions the activation energies for creep of single metal crystals and polycrystalline aggregates and for grain boundary shearing should be identical. This paper is primarily concerned with the possible identity between the activation energies for high temperature creep of single crystal and polycrystalline metals. In addition, comparisons will also be made between the activation energies for creep of single crystals and polycrystals with previously reported activation energies for grain boundary shearing.0"8 Materials and Techniques The same high purity aluminum, lead, and tin were used in the creep tests for single crystals and polycrystalline aggregates. Single crystals of aluminum and tin were prepared by the strain-anneal technique, whereas lead single crystals were prepared by growth from the melt. The tensile creep stress was maintained constant by Chalmers-Andrade parabolic-type lever arms. Strains were measured to &0.0002 in. per in. with rack and pinion type extensometers, and temperatures were maintained to within & 0.2"C of the reported values by mercury-thermoregulated resistance-heated silicone oil baths. The previously reported unambiguous technique for determination of the activation energy for creep was employed throughout this investigation.&apos; ." It involves periodic abrupt small changes in temperature during the course of creep, accomplished by rapidly replacing one creep bath at temperature TI by a second bath at T,. The abrupt change in creep rate from i, to & attending the abrupt change in temperature is due exclusively to the change in temperature, since both the stress and the substructure are identical the instant before and the instant after a change of temperature. Therefore, all other factors being identical where AH is the activation energy for creep and R is the gas constant. Results Typical examples of the creep rate vs creep strain data during temperature cycled creep tests of single

Jan 1, 1958

By E. E. Donath

THE coal hydrogenation process is well known as a means for production of liquid fuels from coal. In this paper, the possibilities of the coal hydrogenation process as a source of chemical raw materials will be discussed. The recovery of chemicals from coal hydrogenation products necessitates some modifications and additions to the equipment used for the production of fuels. The conversion of coal into liquid fuels such as gasoline requires two steps: liquid-phase and vapor-phase hydrogenation. Intermediate oils obtained in the liquid phase contain oxygen and nitrogen compounds, especially aromatic compounds, since the coal itself is composed mainly of cyclic compounds. These oils are the raw material for the separation of high-molecular-weight aromatics and of tar acids and tar bases. The relative amounts of heavy and middle oil-boiling above and below 325ºC, for instance-can be influenced by temperature, residence time, and catalyst of the liquid-phase hydrogenation. In vapor-phase hydrogenation, a solid bed catalyst is used to convert the intermediate oil from the liquid-phase operation into hydrocarbons of the gasoline boiling range. Essentially pure hydrocarbons with a low content of sulphur, oxygen, nitrogen, and olefines are obtained. Depending mainly on the catalyst, the high ring-compound content of the liquid-phase oil can be preserved and gasoline rich in aromatics obtained. However, with other catalysts, these ring compounds can be split into gasoline with a high content of isoparafhns.3 Again, depending on the operating conditions, products of varying boiling range can be obtained. Selection of catalyst and operating conditions therefore makes possible the production of different grades of motor fuel and also variations in the relative amounts of benzene, toluene, and xylene when aromatic hydrocarbons are produced. The schematic flowsheet, Fig 1, shows the main steps of the coal hydrogenation process, and the product streams used for the recovery of chemicals are indicated. In the liquid-phase stage, coal is made into a paste with re- cycle heavy oil. The coal paste is mixed with hydrogen and preheated at a pressure of 300 to 700 atm in heat exchangers and preheaters. The coal paste and hydrogen enter high-pressure converters where the liquefaction of coal, conversion of the high-boiling liquid materials initially obtained, into intermediate oils is performed at a temperature around 470ºC. The reaction products enter the hot catchpot in which oil vapors of lower boiling point

Jan 1, 1953

By Daniel Kim, Michael Free, Justin McAllister, Urian Marshall, Shijie Wang

"Cathode impurity levels of electrorefined copper were evaluated based on 1/10* scale laboratory electrorefining tests. Cathodes were evaluated near the top, mid-section, and bottom sections of cathodes on both the set and mold sides and strip and scrap cycles. Slime weights were measured, and slime and electrolyte samples were also evaluated for impurities. Results from these tests have been compiled and compared to evaluate the effects of changes in operating conditions and electrode location on cathode impurities.IntroductionMany types of impurities are commonly found in commercial copper electrorefining anodes. The smelter operations that produce the anodes process concentrates that contain a wide variety of impurities that vary based on the mineralogy of the ore. Most anode impurities are removed during electrorefining. However, a portion of the anode impurities is incorporated into the copper cathode product. The mechanisms by which impurities are transported from the anode to the cathode are not well understood. Some impurities can be transported as anode slime particles to the cathode where they are incorporated into the cathode. Other impurities can be transported as dissolved species that are electrochemically reduced with the copper to become part of the cathode. Although research has been performed on anode slimes and impurities [1-4], there is a need for additional information regarding the relationships associated with electrorefining cycles, electrode faces, local electrode positions, anode impurities and specific cathode impurities. The objective of this study was to evaluate lead, arsenic, and antimony cathode impurity trends associated with electrorefining cycles, electrode faces, local electrode positions, and anode impurities. A variety of techniques including electrolyte filtering, anode heat treatment, high electrolyte arsenic concentration, high arsenic and/or lead in anodes, flocculation of slime particles, and appropriate current density control were used to vary cathode impurity levels. Each test was performed only once for a strip cycle and once for a scrap cycle. Consequently, the results for the individual conditions are preliminary and are not the focus of this study. However, the collective set of data with varying impurity modifying techniques provides a broad range of impurity levels, and the associated trends with respect to lead, arsenic, and antimony are discussed in this paper. Approximately 180 analyses of copper cathode were used to track the antimony, arsenic, and lead impurities. Eighteen anode slime samples were also analyzed for antimony, arsenic, and lead."

Jan 1, 2012