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By Noriaki Kurita, Norihiko Fulcatsu, Teruo Ohashi

"An electrochemical sensing device for hydrogen in molten metal has now been available owing to the development of the proton conducting solid electrolyte made of ceramics of metal oxide. The structure of the sensor and the theoretical limitations of its applications are discussed based on the electrochemical properties of the electrolyte used. The practical performance of the sensor is reviewed from the results of test measurements at the plants of aluminum and copper melting industries. The effectiveness of the sensor to the process control of continuous casting of copper is also discussed.IntroductionSince the in-line monitoring of the amount of oxygen dissolved in molten metal was realized by using the oxygen concentration cell based on zirconia solid electrolyte a similar method has been expected to be developed for sensing of hydrogen, which is a very important element of gas species in liquid metals, especially, in aluminum and copper. In 1981; Iwahara and coworkers found the dominant proton conduction at a high temperature in some perovskite-type oxide (1). Since then, the effort has been made to apply this proton conducting material as the electrolyte of the hydrogen concentration cell for high temperature use. The hydrogen sensor for liquid aluminum of this kind was first produced in 1991 (2) and released commercially from TYK Co., Ltd. Recently, we have developed the mother one usable at higher temperature such as copper and silver melting processes (3). In this note we discuss their structure, design and applicable limitations based on the electrochemical properties of this new type electrolyte. The performance of the sensor and benefit to use it to control the melting process is also discussed"

Jan 1, 2000

By Singareddy R. Reddy, Ramana G. Reddy

"The Margules equation is used for interpreting excess Gibbs energy of several ternary systems. An expression for the activity coefficient of a dilute solute, 2(oxygen), in a binary solvent 1-3 is derived. It is used to calculate the logarithmic activity coefficient of oxygen in Pb-O-Gu, Pb-O-Bi, AgO- Sn, Pb-O-Sn and Ag-O-Pb metallic systems. Self interaction parameter of the solute is derived from the partial Gibbs energy of solute using constant compositional path. The derived equation is used successfully to deduce the self interaction parameter of oxygen in Pb-O-Gu and Pb-O-Bi metallic systems. The predicted thermodynamic parameter data i.e activity coefficient and self-interaction parameters are in an excellent agreement with the experimental data and also our predictions are far more accurate than the predictions made by other models.1 IntroductionThe nature of solute interactions such as oxygen, nitrogen and sulfur with the metallic solutions are important for a number of chemical and metallurgical processes. Several theories [1-23] have been developed to evaluate fundamental thermodynamic properties of solutes constituting two elements. The activity of solutes has been calculated using statisticalor quasi- chemical approach.Wagner's [4] Ideal Solvent Model is based on one energy parameter to describe the compositional dependencies of the activity coefficient of nonmetallic solutes such as oxygen in binary metallic solutions. This model depends on a constant energy of interaction for the exchange of atoms from the coordination shell of an oxygen atom to the shell of an interstitial site and cannot account for properties of strongly interacting systems [4]. Therefore, several attempts have been made to improve the Wagner's model for the strongly interacting systems. [10-16]."

Jan 1, 1996

By W. K. Collins

Engineered Scavenger Compounds (ESCs), developed by the U.S. Bureau of Mines, are a novel class of compounds that can selectively recover a desired element from a solid or molten alloy. Lithium titanate (Li2Ti3O7 or L'20-3T'02) is being used as an ESC to recover lithium (Li) from Aluminum-Lithium (Al-Li) alloys. X-ray diffraction measurements have shown that lithium titanate undergoes a phase change from an orthorhombic structure to a hexagonal structure. This change is due to the incorporation of Li in the matrix of the material and the effect of temperature. Although both are metastable, the hexagonal phase that forms during the scavenging of Li from Al-Li alloys appears to be the more stable phase. Recovering Li from the ESC by electrodeposition does not cause the structure to revert to the orthorhombic phase. Both the orthorhombic and the hexagonal structures of Li2Ti3O7 have similar scavenging capacities for Li. This paper proposes a new mechanism for the phase transformation.

Jan 1, 1993

By K. Fagerlund

Methods for simulation of settler reactions, matte-slag separation and matte settling in copper flash smelting have been examined. The reaction, separation and settling phenomena of slightly oxidized chalcopyrite samples and cuprous sulfide-magnetite mixtures in fayalite type slags were examined at about 1300°C under inert atmosphere. Two methods based on introduction of molten samples of oxidized chalcopyrite concentrates or synthetic matte-magnetite mixtures onto the surface of molten iron silicate slag were tested. In the first method the samples were water quenched and polished specimens were studied and analysed using light optical microscope, scanning electron microscope, energy dispersive spectrometer. In the second method processes taking place after the introduction of samples onto the slag are followed "in situ" using X-ray transmission image monitoring. Great differences were observed in separation and settling behaviour of low and high grade copper mattes produced as a results of interaction of initial samples and slag.

Jan 1, 1997

By Chunlin Chen

Nickel-sulfide minerals are normally associated with copper and iron sulfides and often contain a minor amount of valuable metals such as cobalt and detrimental impurities such as arsenic. Metal losses in slag vary from process to process during the pyrometallurgical production of nickel and, depend on the feed composition, slag chemistry and operating conditions. Maximiz the metal recovery is one of major considerations to optimize operating condition for nickel smelting/ converting processes. At the same time, the deportment of minor elements between various phases during nickel smelting is of great importance by smelter operators. The Multi-Phase Equilibrium (MPE) is a thermodynamic package developed by CSIRO for simulating reactions between phases in multi-component and multi-phase systems [1]. Over the years the capability of the MPE model has been extended to cover the behavior of a large number of elements in high temperature systems. The sulfide smelting module of the MPE, which covers the minor elements such as As, Bi, Sb, Pb, Se, Te, Sn, Co and Zn, is capable of modeling the deportment of major and minor elements between various phases during nickel smelting. In this article the application of the MPE model in modelling the nickel smelting process is presented. The modelling results on the majors and minors are compared with the plant data. The deportment behaviour of arsenic in nickel smelting was analysed and the impact of slag chemistry on slag properties was modelled. These results can assist process metallurgists in exploring the optimum fluxing strategy for smooth operation and the potential practices for improving arsenic removal.

By B. Mishra

Calcium and lithium gallides have been synthesized by powder metallurgy techniques in the stoichiometries that can be used as reduction alloys for the Rocky Flats Plant Salt-Scrub (SS) process. The SS process is performed to recover valuable metals from salts generated in the electrorefining and the molten salt extraction processes. Combustion synthesis has been optimized for variable heating rates up to the reaction ignition temperature and for green densities of the powder compacts in terms of the ignition temperature and the exothermic heating of the product in an effort to develop LiGa and CaGaz alloys. The problems arising from the melting point and density differences of calcium, lithium and gallium have also been studied. The SS alloy compositions were produced by mixing, pressing and sintering the metal-powders. The efficiency of the intermetallic alloy, Ca-17 wt. pct. Ga, as a reductant and the effect of gallium on salt clean- up has been discussed. Measurement of actinide recovery has been studied with cerium as the surrogate for the actinide metal. The development of an alloy for SS reduces a major contaminated waste disposal problem besides recovering the valuable reactive metal.

Jan 1, 1993

By Batric Pesic

The interactions of mineral-pyrite with T. ferrooxidans were studied by using a cyclic voltametry technique. The interactions with bacteria were examined during the entire growth stage of bacteria (fermentation), The pyrite ?surface invariably drastically changed ' its. properties at the second day of fermentation. Beyond two .. days of fermentation, the cyclic voltamograms were insensitive to convective diffusion produced by stirring. The product layer was examined by SEM,. X-ray diffraction and chemical analysis. The SEM study revealed that bacteria populated the pyrite surface at an extremely high density levels. The high density of bacteria, and the solid reaction products formed on the pyrite surface created conditions for pore diffusion which explained why the CVs became .insensitive to convective diffusion in solution (stirring). The x-r:ay diffraction study confirmed jarosite as a product layer. A mechanism of T. ferrooxidans cells serving as nucleation sites for jiarosite formation is proposed.

Jan 1, 1991

By Hongbo Zhu, Jinhui Peng, Linqing Dai

"To optimize the process variables for making direct reduced iron (DRI) by microwave heating, the reduction temperature, reduction time and the ratio of coal to material were studied with the central composite design (CCD) and their interactions on the Metallization rate were also investigated. The predictive polynomial quadratic equations model was analyzed by ANOVA. Optimal conditions of making DRI can be concluded as follows: 28 min at 1139?, the ratio of coal to material is 20.95%. Under these conditions, the metallization rate is up to 97.06%.1. IntroductionThere are some technical problems in making direct reduced iron (DRI) or sponge iron using iron ore concentrates containing coal and lime. In reduction of the iron ore concentrates containing coal with microwave heating, the strength of pellets needn’t to be considered. It reduces the costs and improve quality of materials, but also eliminates the need for pellet preparation process, simplifying the process and achieving a cleaner production.Microwave energy is a clean energy, and has characteristic of selective heating. The speed of heating is also fast. It researched by Chen Jin that when the mole mass of C: O is 0.627 and the microwave power is 15KW, it only spends 15min from 15? to 1021.6? with 1 kg iron ore containing coal with microwave heating [1]. There are many factors affecting metallization rate. In order to find a suitable condition for reduction process, it is necessary to design a series of suitable experiments.Response surface methodology (RSM) is one of the relevant multivariate techniques which can deal with multivariant experimental design strategy, statistical modeling and process optimization [2–5]. It is used to examine the relationship between one or more response variables and a set of quantitative experimental variables or factors. This method is often employed after the identification of the vital controllable factors to find the factor settings that optimize the response. Designs of this type are usually chosen when a curvature in the response surface is suspected. The process optimization of the microwave reduced iron ore was seldom reported in literature. Hence the present work intends to assess the effects of variables such as reduction time, reduction temperature and the ratio of coal to identify the optimum conditions using a central composite design (CCD). The characteristic of product was assessed using scanning electron microscope (SEM)."

Jan 1, 2011

By M. A. Gimenes

The utilization of chlorination in extractive metallurgy and advanced ceramics areas has been widely investigated as a preparative route in order to obtain intermetallic compounds, which are used as precursors in the development of new materials and process. The major processes of decomposition of rare-earth ores use sulfuric acid and sodium hydroxide at high temperatures, however there is not much work concerning chlorination. In this work, a systematic study of the reaction between xenotime (REPO4), chlorine and carbon has been performed. Particular emphasis was on kinetic studies to establish optimized conditions for the reaction. The kinetics of chlorination of xenotime raw material by rare-earth elements/compounds has been studied over a temperature range from 600°C to 950°C. The influence on the rate of conversion of xenotime to RECl3 on temperature, partial pressure of chlorine, carbon content, and particle size were investigated. A global rate equation that includes these parameters has been developed. The results show that the process follows the unreacted core-shrinking model with a formation of a porous product layer. The powder X ray-diffraction technique corroborated this model showing clearly the patterns related to the formation of yttrium oxychloride (YOCl), indicating that the reaction mechanism involves the presence ofan intermediate step before the formation of lanthanide chloride.

Jan 1, 2000

By L. A. Harris

In the present study the open gradient magnetic separation' (OGMS) method has been used to beneficiate the -30 + 100 mesh fraction of two high volatile bituminous coals. The evaluation of the effectiveness of the magnetic separation for cleaning these coals is the subject of this paper. Coal petrography in combination with scanning electron microscopy (SEM) and x-ray diffractometry (XRD) were used to characterize the magnetically separated coal fractions. These analyses revealed that the majority of the pyrite and non-pyrite minerals were concentrated in the positive magnetic susceptibility fractions. The bulk of the starting samples (-80 weight percent) were located in the negative magnetic susceptibility fractions and showed significant reductions in pyrite and non-pyritic minerals. The magnetic separation appears to effectively split the samples into relatively clean coal and refuse.

Jan 1, 1981

By John B. Cocanour

The U.S. Bureau of Mines (USBM) has developed a laboratory-scale on-line analysis and process control system for a decopperization electrolytic circuit. This system is software driven, running on a 486DX-33 personal computer (PC) utilizing a portable energy- dispersive x-ray fluorescence (XRF) spectrometer as the sample analyzer. The XRF copper reading obtained was used as the control variable through an RS-232 serial interface to the PC for software-based control of feed flowrates. When the copper concentration in the electrolytic cell (as measured by the XRF) deviated from the set point, the feed flowrate to the cell was automatically altered using software-based proportional-integral-differential (PID) computer control to yield the desired copper concentration at the electrolytic cell outlet.

Jan 1, 1994

By C. Burton Clark

The important role of the petrographic microscope in the petrology of refractories is discussed, based on 45 years of industrial experience by the author. Highlights of his career are used to illustrate improvements in equipment and techniques during the period. Two specific investigations are described which emphasize the interrelated use of the petrographic microscope with other instruments such as the x-ray diffractometer and scanning electron microscope. Emphasis is placed on the use of phase equilibrium diagrams for guidance in predicting and interpreting reactions that occur under non-equilibrium conditions in the manufacture and use of refractories.

Jan 1, 1982

By Jim A. King

The total pressure oxidation of copper concentrates is a potentially viable option for treating copper concentrates that are either low grade or contain significant impurities. Both concentrate types are heavily penalized in smelter contracts. The total pressure oxidation process involves autoclaving the copper concentrate at temperatures of 200-220 C under oxygen pressure. The autoclave discharge can be separated into a solid (oxidation residue) and a liquid (oxidation solution) product. The oxidation solution can be treated for copper recovery by solvent extraction - electrowinning or by direct electrowinning. The direct electrowinning recovery of copper requires prior removal of selenium and tellurium by cementation on finely divided scrap copper. The oxidation residue is washed thoroughly to remove acid and dissolved copper prior to precious metals recovery by conventional cyanidation in the presence of lime. The results of a benchscale investigation involving a number of copper concentrates are reported. Copper recoveries in autoclave oxidation and gold recoveries by cyanidation of the oxidation residue exceeded 99%. The results of benchscale experiments to demonstrate copper recovery are described. Various flowsheet options are presented.

Jan 1, 1993

By V. A. Luganov

The behavior of arsenopyrite under heating has been studied by many scientists. It has been already established that under heating at more than 650°C and without air access the arsenopyrite dissociates with the formation of one atom arsenic. Under vacuum the dissociation process begins at 550 DC with the formation of elemental arsenic. The residue of dissociation process contains pyrrhotite and throilitc. In the presence of pyrite, arsenopyrite dissociates under lower temperature and with a higher velocity than without it. The industrial realization of fool scale processing of arsenic bearing raw materials is possible only by the use of standard equipment and oxygen containing blast In this view the paper presents the results of the study on the effect of oxygen in the gaseous phase and its addition into the charge of pyrite in the process of arsenopyrite decomposition. Thermodynamic analyses showed that under thermal processing of arsenopyrite in the presence of pyrite and limited quantities of oxygen in the gaseous phase the formation of arsenic sulfides is possible according to the following reactions:

Jan 1, 2003

By H. L. Fraser

A review of the possibilities of performing microchemical analysis in thin sections using a combination of scanning transmission electron microscopy and energy dispersive spectroscopy of x-rays is given. Particular attention is paid to the factors that limit accurate analysis at the highest spatial resolution. As an example of the use of these techniques applied to a potential problem in minerals processing, the identification of iron pyrite and pyrrhotite particles in Illinois, Herrin #6 coal is presented.

Jan 1, 1981

By Adriana de Aquino Soeiro da Silva, Joao Alves Sampaioa, Luiz Carlos Bertolino, Francisco Manoel Garrido, Marta Eloisa Medeiros

"Brazil has a large agricultural potential and its production success is related to the chemicaland physical soil characteristics. Therefore, the demand in the use of a great quantity offertilizers to compensate the low amount of nutrients in the soil includes about 40% of foodproduction costs. In order to develop economical alternatives to traditional fertilizers, rockswith potential use in agriculture will be studied. In this work the potassium rock, a greensandslate, will be chemically and structurally characterized for the development of a potassiumthermophosphate. This alternative fertilizer will be obtained based on a fusion of a ponderedmixture of potassium, magnesium and phosphate rocks to be applied in the Brazilianagriculture. Preliminary characterization results indicate that the greensand slate presents ahigh percentage of glauconite, quartz and micas.Keywords: Potassium thermophosphate, alternative fertilizers, greensand slate.IntroductionBrazil has a great agricultural potential and its production success is closely related to thesoil's chemical and physical characteristics. However, the country's soils present lownutrients content and high acidity due to weather conditions. Thus, the use of a high amountof fertilizers makes up for the soils' lack of nutrients and accounts for 40% of food productioncosts. Therefore, research on obtaining new alternative fertilizers is a constant worry due tothe increase on food demand [ 1].The lack of raw material for the preparation of NPK fertilizers in Brazil is a concern and theissue of potassium fertilizers a priority. Such a fact is because in 2008 only 608.000 tons ofKCl were produced, corresponding to just 10% of the Brazilian necessity. Thus, the use ofrocks as agricultural nutrients can contribute to reduce the need for industrial fertilizers.This way, the development of a new agricultural raw material originated from a rock thatalready exists in the country's soil is of great importance for the mineral and agriculturalsectors."

Jan 1, 2011

By Do-Hyeong Kim, Tae-Jung Kim, Seung-Yeon Won, Jong-Jin Pak, Min-Kyu Paek

Liquid iron alloys containing V, Mo, and Ni can be produced by the carbothermic reduction of spent catalysts used in petrochemical industry. Thermodynamics of carbon in these alloy melts is important for refining these alloys. In the present study, the carbon solubility in Fe-V, Fe-Mo, Fe-Ni, Fe-V-Mo, Fe-V-Ni, Fe-Mo-Ni and Fe-V-Mo-Ni alloy melts of various compositions was measured at 1873 K. The temperature dependency of vanadium effect on carbon solubility in liquid iron was also measured in the temperature range from 1823K to 1923K. The additions of vanadium and molybdenum significantly increased the carbon solubility in liquid iron alloys while nickel decreased the solubility. The experimental results were thermodynamically analyzed using Lupis’ relation at constant activity to determine the first- and the second-order interaction parameters of vanadium, nickel and molybdenum on carbon at carbon saturated condition. Using thermodynamic parameters determined in the present study, the carbon solubility in Fe-V-Mo-Ni alloy melts of various composition were accurately predicted and verified experimentally at 1873 K.

Jan 1, 2014

By K. Morsi, S. K. Kassegne, A. El-Desouky, K. S. Moon

"Current Activated Tip-based Sintering (CATS) is a new process for the powder-based fabrication of macro, micro and possibly nano-scale features and shapes. This new and unique process enables selective sintering of powders by localizing electrically activated sintering conditions through a stationary or moving electrically conducting tip. We present preliminary experimental results on the effect of tip size in the CA TS process as well as the effect of initial powder particle size on the sintering behavior of nickel powder.IntroductionSpark Plasma Sintering (SPS) has been the center of attention of numerous researchers due its noticeable advantages over conventional sintering techniques such as rapid heating rates, lower sintering temperature and shorter holding times. Research on SPS has been applied on a wide variety of materials such as pure metals [ 1], ceramics [2], composites [3], nano-materials [ 4], biomaterials [ 5], shape memory alloys [ 6] and many other material systems. However, it has been mostly limited to bulk materials with simple shapes with a few exceptions ofresearch efforts where the effect of electric current was combined with metal forming processes such as spark plasma extrusion [7,8] and electric rolling of powders[9]. In this paper a novel process (Current-Activated Tip-Based Sintering (CATS)) is discussed where electric current and pressure are applied simultaneously through a small conducting tip (stationary or moving) over a conducting powder compact. This process has the potential advantages of sintering complex geometries with minimum energy requirements as unconventionally high current densities can be achieved due to the small contact area between the tip and the powder compact. Furthermore, by controlling the tip size, it can be possible to sinter features on the macro-, micro- and even nanoscales."

Jan 1, 2011

By W. D. Keller

Scanning electron microscopy (SEM) accompanied by X-ray energy dispersive analysis (XES) is a useful tool in process clay mineralogy. The texture of kaolin, illustrated by SEM, gives a clue to its mode of genesis and probable industrial application. One type of kaolin, originating dominantly by weathering, has an open texture, slakes readily, and is used for filling and coating paper. Another type, in contrast, originates by diagenesis of Al-silicate sediments, and spectacularly resists slaking, thereby enabling it to maintain its bulk density and controlled size and shape of particles after crushing and moistening; this meets an important requirement for the manufacture of refractories. Ratios of elemental Al:Si that may be rapidly determined by SEM and XES yield information on the origin and purity of bauxite and bauxitic clays, and aid in quality control and processing of them. SEM of dissimilar textures of quartz, as in chert and novaculite, are evidence for geothermometry on a stratigraphic scale that is potentially useful in delimiting thermally favorable or unfavorable areas for hydrocarbon exploration, and possibly for unexposed metallic ore deposits.

Jan 1, 1982

By R. J. Mitchell

Results from investigations into impurity distributions over cathodes are presented with implications for various sampling methods, Selection of an optimum treatment procedure for the test sample is outlined. The impact of both these studies on the development of an in-house method for sampling Isa Process cathode is discussed. The economic compromise actually undertaken, satifying wants and needs to sustain confidence in high grade cathode purity is detailed.

Jan 1, 1987