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By Shulan Wang, Xuan Liu, Li Li

"Electrochemistry of Fe(III) in 69CaCl2-12CaF2-19KF and 81CaCl2-19KF (mole percentage, %) was investigated at 827 oC on molybdenum electrode by cyclic voltammetry, chronoamperometry and galvanostatic electrolysis using Fe2O3 as the Fe(III) source. The reduction of Fe(III) to Fe was conducted in one step and controlled by diffusion process. Fe(III) shown greater reduction rate and diffusion coefficient in molten 81CaCl2-19KF than in 69CaCl2- 12CaF2-19KF. Galvanostic electrolysis of Fe was performed in both molten salts with a cylindrical cathode rotating at 200 r/min and dendritic iron deposit was obtained.Keywords: iron; electrolysis; electrochemistry; molten saltIntroductionThe production of iron and steel causes huge emissions of CO2. Iron electrowinning in molten salts with dissolved Fe2O3 using an inert oxygen evolving anode is an alternative process to reduce or eliminate the formation of CO2. Research on novel process of producing metal has been reported recently [1-2] by using CaCl2 as the main electrolyte and dissolving CaO in CaCl2 due to the high solubility of CaO in the melt. This process has been used in preparing many active metals and alloys [3-14]. In the present work, the electrochemical behavior of iron in CaCl2-KF was studied and transport property of iron ion in the melt was discussed.ExperimentalCaCl2,CaF2 and KF (in analytical purity) were dried in air for 48 h. Mixed salts used in experiments were placed in a graphite crucible (??58 mm inner diameter). The graphite crucible together with the salts was heated at 473 K for 12 h in a furnace with flowing Ar (99.99%) before further heating. Temperature inside the furnace was measured by an S type thermocouple. Electrochemical measurements, such as cyclic voltammetry and chronocoulometry, were performed in a three electrode cell by EG&G PAR273A potentiostat/galvanostatand. Galvanostatic electrodepositon of iron was conducted in a two electrode cell. Molybdenum (??2 mm) and iron (??5 mm) were used as the working electrode (WE) and the reference electrode, respectively. A graphite crucible and a magnetite rod (??25 mm ) consisted of 100% magnetite and sintered at 950 oC in argon atmosphere for 2 h with electrical conductivity of 366 O-1m-1 at room temperature were used as the counter electrodes in the galvanostatic electrolysis experiment. Carbon (??10 mm) was used as the counter electrode in electrochemical measurement. The deposits were washed in distilled water bubbled with argon and dried in air before being characterized by X-ray diffraction (PW3040/60 diffractometer) and scanning electron microscope (SEM, SSX-550)."

Jan 1, 2014

By He Zhi-jun, Ning Zhe, Pang Qing-hai, Zhang Jun-hong, Zhan Wen-long

The effect of microwave irradiation on grinding property of coal was studied by using Hardgrove grindability index tester. Superior grindability of coal was obtained to varying extent after microwave irradiation treatment. The variation in microstructure of pulverized coal during microwave irradiation was observed by utilizing scanning electronic microscope (SEM). The results indicated that the different microwave absorbance of minerals and carbon matrix led to cracks on their interface, by which coal particles were further pulverized and therefore the granularity of coal powder was reduced. Due to the different formation process of various coals, bituminite and anthracite are very different in physical and chemical properties. According to the content of coal pulverization, it can found that microwave irradiation has a stronger pulverizing effect on bituminite in comparison to anthracite.

Jan 1, 2016

By María Guadalupe Sánchez-Loredo

Silver from nitrate aqueous solutions was extracted by commercial organophosphorous extractants (tri-n-butylphosphate, Cyanex 471x, Cyanex 301 and Cyanex 302). Quantitative silver extraction was obtained using the Cyanex reagents. After loading, aqueous solutions of several reducing reagents were used to prepare fine silver powders by reductive stripping. Only both extractants Cyanex 471x and tri-n-butylphosphate (TBP) could be reductive stripped and regenerated by aqueous solutions of ascorbic acid, and Cyanex 471x was decomposed to the corresponding phosphine oxide by using sodium borohydride as reducing agent. Silver was recovered as fine particles, which were characterised by means of scanning electron microscopy (SEM). Micrographs showed that the powder size and morphology were directly affected by the composition of the applied organic phases and aqueous reducing media.

Jan 1, 2003

By David G. Dixon

From its first implementation for the recovery of gold from low-grade ores by cyanidation in the early 1970s, heap leaching has developed into a key hydrometallurgical technology, in conjunction with solvent extraction and electrowinning, for the recovery of base metals, including most notably copper from both oxides and secondary sulphides, and more recently, nickel and zinc. And, given recent advances in bioleaching with thermophilic microbes, the successful application of heap leaching technology to low-grade primary copper ores seems only a matter of time. However, with each new development, it becomes increasingly apparent that the successful application of heap leaching technology will ultimately depend on our having an ever more complete understanding of the fundamental processes underlying it. Much work has been done toward the development of this understanding, on many different fronts. In this paper, a critical overview of heap leach modeling work to date is presented in terms of the most important phenomena which occur during heap leaching, and potential directions for future work are discussed.

Jan 1, 2003

By S. Bagchi

The LaNi5-xMnx-hydrides have potential applications in cryocooling devices for non-mechanical method to compress hydrogen gas. Thermal aging behavior of LaNi5-xMnx-hydrides of compositions x=0.4 and x=1.5 has been investigated. The hydriding properties of the La1.02Ni4.6Mno.4 alloy do not change significantly after thermal aging at 453K for 260 hours. X-ray diffraction analyses of this aged alloy do not reveal the presence of any new phases but the Bragg peaks become broader. Line profile analyses show anisotropic microstrains with an average <e2>1/2 value of -5x103. Thermal aging of the other hydride, LaNi3.5Mn1.5 hydride, at 623K for 280 hours, showed significant disproportionation; the hydrogen capacity reduced significantly from an H/M value of 0.75 in the activated condition to -0.15 after aging. X-ray diffraction analyses showed disproportionated lanthanum dihydride, metallic Ni, and Mn phases. The Bragg peaks were very broad indicative of microstrains or small crystalline domains.

Jan 1, 1997

By Carole Read

Hydrogen is under consideration by several countries for its potential as an energy carrier for transportation applications. In order to compete with vehicles in use today, hydrogen-powered vehicles will require a driving range of greater than 300-miles in order to meet customer needs and expectations. For the overall vehicular light-duty fleet, this dictates that a range of 5 to 13 kg of hydrogen be stored on-board (assuming a fuel cell power plant) within stringent system weight, volume, and cost constraints. Vehicular hydrogen storage thus constitutes a major scientific and technological challenge. To meet this challenge, the U.S. Department of Energy (DOE) initiated a ?National Hydrogen Storage Project? with roughly 40 universities, 15 companies and 10 federal laboratories, actively engaged in hydrogen storage research. Centers of Excellence in metal hydrides, chemical hydrides, and carbon-based materials have been established, as well as independent university and industry projects in the areas of new concepts/materials, hydrogen storage testing, and storage system analysis. Recent technical progress in each of these areas is discussed, as well as collaborative hydrogen storage activities under the recently established International Partnership for the Hydrogen Economy (IPHE).

Jan 1, 2006

By Wenying Liu

The effect of aeration on chalcocite heap leaching was studied by analyzing the historical data from two chalcocite heap leach pads located in Chile, one with aeration and the other without aeration. The data showed that the copper leaching kinetics of the aerated heap was greater than that of the unaerated heap within a certain leaching period, after which there was no effect of aeration on the copper leaching kinetics. The total acid consumption per ton of ore processed was higher in the case of aeration, which was supported by the higher pH of the PLS. But the net acid consumption per ton of copper produced was the same in the two cases. Approximately 5% of the total iron added to the unaerated heap was precipitated inside the heap. In contrast, there was no net iron precipitation or generation inside the aerated heap. Bacteria activities were thought to occur even in the unaerated heap, but the extent was much less than in the aerated heap. Given the importance of forced aeration in chalcocite heap bioleaching, mathematical modelling will be applied in the future work to assist the optimization of the aeration system design.

By Wei Yin, Bin Xu, Qian Li, Yongbin Yang, Tao Jiang

Copper anode slime is an increasingly significant resource for precious metals such as Au, Ag and Pd. The extraction of Au, Ag and Pd from decopperized anode slime by different pretreatments and different lixiviants including cyanide, chloride, thiourea and thiosulfate have been investigated. When oxidizing roasting pretreatment was carried out under the conditions of roasting time 120min and temperature 625 ℃, the removal ratios of S and Sb could reach 82.18% and 98.52%, respectively. And the following alkaline leaching of calcine could result in the dissolution of 46.40% Cu and 98.48% Pb. The optima leaching ratios of Au, Ag and Pd reached 99.48%, 97.69%, 94.79% by cyanide leaching, and 95.01%, 79.84%, 96.59% by chloride leaching, and about 95.21%, 95.66%, 48.79% by thiourea/thiosulfate leaching.

Jan 1, 2015

By Carla Lupi

In this work, nickel-cobalt electrodeposition under galvanostatic conditions was investigated. Ni-Co alloy was electrowon from an acid sulphate bath containing 40 g/L Ni and2-8 g/L Co.. The effect of electrolyte composition, current density, temperature, solution pH and presence of buffers such as H3BO3 and (NH4)2SO4 on Co content of the binary alloy has been investigated. In particular, current densities ranging from 180 to 400 A/m2 and temperatures ranging from 27 to 60°C were tested. The composition of Ni-Co alloys may be diversified through the selection of process parameters. The experiments show that the highest cobalt content of the alloy is reached by using a buffer free electrolyte without solution pH control. Though, in these conditions, the most homogeneous, fine and regular deposit morphology is obtained, energy requirements are the highest in tests lasting just two hours.

Jan 1, 2003

By Adam Gesing, Paul Marchwica, Jerry Sokolowski, Sharon Lackie

"Often referred to as SEM-EDX, energy-dispersive spectroscopic analysis of characteristic fluorescence x-ray is a standard technique for semi-quantitative elemental composition analysis in scanning electron microscopy. It is quick and extremely useful for identification of phases in the sample microstructure, as long as the constituents are significantly larger than the probe volume from which the fluorescence x-rays originate. The probe volume ranges from a few to several microns, depending on the electron beam spot size and the acceleration voltage. We report on a new variant of an EDX technique developed to overcome this limitation and allow quantitative elemental analysis of smaller phase constituents, down to a size of several nanometers. This variant involves the calculation of compositions of individual phases from multiple analyses of areas containing phases of interest. This significantly increases the usefulness of EDX for quantitative analysis of new nano-structured materials.IntroductionIn any elemental micro-analytical method, the sample material is illuminated by a probe beam that excites an interaction volume of a sample to emit a characteristic signal. This signal in turn interacts with the sample material through absorption and fluorescence mechanisms before a portion of it is collected by a suitable detector and analyzed for elemental composition. The spatial resolution of the method depends on the minimum interaction volume between the probe beam and the sample material.Laser light beams can be tightly focused to a spot size limited by the photon wavelength and can be used to sample the surface of any material. In micro-LIBS (laser-induced plasma spectroscopy) a focused laser beam ablates and vaporizes a small volume of material from the sample surface, creating a plasma spark. Spectral analysis of the light emission from the plasma spark allows the semi-quantitative determination of the elemental composition of the material removed from the sample surface. The smallest reproducible craters achieved are ~ 3mm in diameter and a few nanometers in depth. [l]Particle probe beams of ions or electrons can be focused to a diameter of a few nanometers at the point of impact on the sample. Ions sputter the sample atoms from the point of impact, and the sputtered ionized material is analyzed by mass spectroscopy in a secondary ion mass spectrometer (SIMS). [2] This gives SIMS resolution in a nanometer range. SIMS equipment, however, is expensive and not readily available."

Jan 1, 2013

By Carla Lupi, Alessandro Pescetelli

"Spent lead battery recycling still shows few weak points in the achievement of a 100% recycling of different waste matters and by- products arising from the recycling process. Some of said problems are dealing with aqueous streams outgoing the recycling plant, and more particularly, a) the waste waters discarded from the breaking and separation unit, b) purification of the spent electrolyte drained from waste batteries and upgrade to a quality compatible with full re-use by the batteries’ manufacturers, c) purification of the mother liquors discarded in the sodium sulfate crystallization process so to produce a salt of commercial grade. All of the above listed problems have been satisfactorily overcome applying an electrochemical process that, through different process conditions and parameters, is able to remove the harmful impurities that hinder the successful commercialization of such by products, or, at least, that can avoid heavy and expensive treatment plant and operation.IntroductionAlmost 100% of commercial lead and lead alloys produced by secondary lead plants is recycled to the new lead accumulators manufacture. The other by-products and residues produced through the lead recycling process may be classified into two groups:a) matters reusable in the new accumulators production processb) matters produced as a result of various reagents and additives used in the recycling process, to be sold to different market sectorsQuality and saleability of by-products are significant points for the economics of the secondary lead plant operation, because, if said by-products are not saleable, they are just wastes, so offsetting potential revenues, and, at the same time, adding a heavy burden to operating cost, like disposal cost [1]. When looking at a typical, modern lead scrap batteries recovery cycle, it is quite evident that we are still rather far from dealing with a waste-less technology (fig.1).The group a) includes 3 by-products produced through the breaking process: among those matters the polypropylene only usually reaches a standard quality suitable for sale to lead manufacturing sector or to other sectors as well. The other two by-products, electrolyte and separators, do not still reach, through a viable and effective regeneration process, a quality standard sufficient for their re-use in the lead batteries sector ."

Jan 1, 2008

By Tadafumi Adschiri

"Supercritical water can provide an unique reaction atmosphere for synthesizing metal oxide nanoparticles. Due to the drastic change of properties of water around the critical point, including density, dielectric constant and ionic product, the reaction phase with O 2 or H2 gas and the reaction rate and equilibrium can be varied to synthesize new materials or define particle morphologies. In this work, hydrothermal crystallization experiments are performed with several types of flow apparatus that allow convenient manipulation of variables such as temperature, pressure, and residence time. Key features in the flow modes and material preparation are discussed. The proposed supercritical hydrothermal synthesis method has the following desirable features: i) nanoparticles can be produced, ii) morphology of the produced particles can be controlled with small changes in pressure or temperature, and iii) a reducing or oxidizing atmosphere can be applied by introducing oxygen or hydrogen or other gases. An overview of this method is given for functional material synthesis of significant industrial interest including barium hexaferrite magnetic particles, YAO/Tb phosphor fine particles and lithium cobalt fine crystals.IntroductionHydrothermal crystallization, a method of metal oxide formation from metal salt solutions, is typically used at temperatures ranging from 373 K to 473 K. We are developing a new process for hydrothermal crystallizations that uses temperatures in the range of 673 K to 723 K, which is just above the critical temperature of water1 • 8 • In this work, we refer to this process as supercritical hydrothermal synthesis. The supercritical state of water allows one to vary reaction rate and reaction equilibrium by shifting the dielectric constant and solvent density with pressure and temperature. From of our research on material production in supercritical water, we have identified the following specific features of the supercritical hydrothermal synthesis method: (i) ultrafine particles can be produced, (ii) morphology of the produced particles can be controlled to some extent with pressure and/or temperature, and (iii) a homogeneous reducing or oxidizing atmospheres can be provided by introducing gases, such as O 2, H2, H2O 2• and so on.1"

Jan 1, 2000

By Baozhong Zhao

In-situ vitrification (ISV) is a new technology used for treating radioactive, organic and inorganic contaminated soils. In this process, electricity is applied through electrodes buried in the contaminated soil to melt it and form an environmentally stable glass-like solid. The organic contaminants and volatile metals are vaporized during heating up, the non-volatile inorganic elements are dissolved and incorporated into the melt. In present full-scale operation, the ISV process can treat 4 to 6 tons of soil per hour at consumption of about 1000 kwh per ton of soil. In this study, various configurations of electrodes were examined in a mathematical model. The results may be used to optimize the ISV process.

Jan 1, 1994

By M. del C. Ruiz

The extraction of Nb and Ta from a columbo-tantalite of San Luis, Argentina, is being studied by using a pressure reactor and HF as leaching agent. The reagents and products have been characterized by several techniques such as scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDXS), X-ray fluorescence (XRF), X-ray difracction (XRD), surface area (BET) and size particle analysis. Experimental results have shown that the extraction of niobium and tantalum increases with increasing temperature, reaction time and acid concentration. For particle size between +80 and -355 mesh no significant changes are detected. It is also slightly affected by the stimng speed. XRD analysis of the residues did not show formation of new crystalline structures.

Jan 1, 1999

By Munetaka Iwasaki

Nitrogen strongly affects mechanical properties of steel and therefore we may sometimes modify the various processes for its content. Numerous studies based on the results of chemical analysis of quenched samples were reported with a few exceptions of Hot Sievert method. The technique always poses a risk of uncertainty whether the true content of nitrogen in liquid metal is measured or not. In this study vacuum remelting under relatively low pressure was done to enhance gas phase mass transfer. Total pressure of the melt chamber was about 10-3 pa and electron beam heating was used. Mass spectroscopy was used for the direct observation of the rate of denitrization. Nitrogen molecules or atoms were detected by a mass spectrometer set above the melt. Continuous monitoring of the intensity of the fixed mass number may reflect the transfer of nitrogen from the melt to the vacuum. The results of the new and conventional techniques agree, both technique can be verified.

Jan 1, 1999

By R. W. Lee

The first prototype plant using the Imperial Smelting Process commenced operation in 1950. It is timely therefore to review the developments that have occurred with the process over the past half-century. A major advantage claimed initially for the process was its ability simultaneously to recover zinc and lead from bulk concentrates. This has remained a fundamental advantage, but it has been extended by the increasing treatment of secondary materials containing zinc and lead. This has been facilitated by the development of hot briquetting and tuyere injection. These techniques and their impact on the technology of the operation will be described. The other major advantage claimed for the process was its potential to achieve new levels of productivity in the pyrometallurgical smelting of zinc. This has been realised with operating furnaces producing up to 400 t/d of zinc. The technical developments that have enabled this scale of operation will be reviewed.

Jan 1, 2000

By Corby Anderson

The efficient separation of palladium from the transition metals copper, nickel and iron can be effected by passing a leach solution of these metals through a column of the silica polyamine composite material, WP-1, patented by Purity Systems Inc (PSI), Assignee, University of Montana with exclusive license to PSI. The separation can be done at the intrinsic pH of a nitrogen species catalyzed (NSC) oxidative pressure leach solution (~0) and stripping of the palladium from the composite can be effected with hydrochloric acid/ammonium chloride solutions at 50oC. Batch capacities of the composite for palladium are ~ 1.8 mmol/g resin. The possibilities for isolating the metal from the strip are discussed. Given the proven longevity and rapid capture kinetics of the polyamine composites, this new approach should prove to be an economically viable alternative to the multi-step concentration processes practiced in the PGM industry to date.

Jan 1, 2003

By John M. Rapkoch

In the continuing search for copper matte converting methods, commercially available and feasible choices remain Peirce-Smith Converters, Hoboken Converters, Mitsubishi Converting, Ausmelt converting, and Outokumpu/Kennecott Solid Matte Oxygen Converting (?Flash Converting?). While each alternative improves on Peirce-Smith Converters? limited fugitive gas capturing capability, the Peirce-Smith Converter is relatively easy and economic to operate and has an unmatched ability to accept valuable but difficult-to-handle material such as scrap anodes and purchased scrap copper. Recent experience with designing, building, and starting up an ISASMELT facility, applied in primary smelting of copper concentrates, has led the authors to speculate on how suitable the ISASMELT process would be for copper converting, given its low fugitive gas release and its ability to accept a variety of feed types. This paper reviews the potential metallurgical challenges posed by converting copper matte in an ISASMELT vessel and considers possible engineering and design challenges posed by the inclusion of this technology into a new or refurbished copper smelter.

Jan 1, 2006

By S. J. Kohut

Until recently SX-EW technology has only been used to produce conventional cathode for the cyclical commodity marketplace. Unlike electrorefining, SX-EW lends itself to the integration with the downstream manufacturing technologies for direct mine site production of value added products. The integration of SX-EW and downstream manufacturing results in the elimination of redundant process steps, the cost savings, and the access to value added product markets which can buffer the producer from swings in the cathode market. SX-EW production of copper powder and powder-based products has been demonstrated at the pilot plant level. The SX-EW process has been successfully redesigned to meet the more specific demands of engineered products. Challenges include the solution purity, the cell ventilation, the high current density operation and the product handling. Successful demonstration of mine site production of value added SX- EW products opens up new non-commodity marketplaces to the mining industry.

Jan 1, 1999

By Chai Liyuan

This paper focused on the preparation of porous ceramic pellets for microorganism carriers. A new method for the process was developed using simple gel-casting and bubble-in-water-in-oil type of multiphase double emulsion. The globules, consisting of a foamed sepiolite slurry suspension, were dispersed and consolidated in spherical shape in liquid paraffin as gelation progressed. The green pellets were sintered at 1100°C. The influence of surfactants, extension ratio and impeller revolution rate on the process and characteristics of the pellets was investigated. The pellet size was in the range of 1~4mm and determined directly by impeller revolution rate. The fine cell diameter of porous ceramic was in the range of 100~500m and the micropore diameter was less than 5m. The inner macropores were interconnected and extend to the external surface. It is impossible to analyze a result by SEM micrographs and digital camera.

Jan 1, 2006