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By Richard B. Diver, Mark D. Allendorf, Daniel E. Dedrick, James E. Miller, Roy E. Hogan, Andrea Ambrosini, Eric N. Coker, Anthony H. McDaniel, Nathan P. Siegel, Gary L. Kellogg

"Converting carbon dioxide and water to hydrocarbons is an attractive option for storing solar energy and, coupled with appropriate CO2 capture technology, for recycling carbon and impacting atmospheric CO2 concentrations. For any process, high solar-to-fuel efficiency is necessary for large scale viability and favorable economics. Thermochemical approaches for solar-to-fuel conversion are potentially highly efficient as they avoid the inherent limitations of photosynthesis and also sidestep the solar-to-electric conversion necessary to drive electrolytic reactions. Solar-driven two-step metal-oxide-based thermochemical cycles for producing the components of syngas, CO and H2, from CO2 and H2O are the basis of the “Sunshine to Petrol” project. Multi-cycle production of both H2 and CO has been demonstrated over several iron- and cerium-based compositions fabricated into monolithic pieces both in the laboratory and at the National Solar Thermal Test Facility. These compositions are being developed for deployment in a unique and continuous solar-driven reactor prototype, the counter-rotating-ring receiver reactor recuperator or CR5.IntroductionThe interconnected challenges posed by increasing global competition for petroleum and the increasing concentration of atmospheric carbon dioxide are now widely recognized. Meeting these challenges requires recognition that although hydrocarbon fuels are ideal energy carriers, they can no longer be thought of as primary energy sources. It is necessary to take the realistic view that our conventional fossil fuels are in fact “stored sunlight” in the form of “sequestered carbon.” This view leads to a search for options to use and store sunlight more directly.Sunshine to PetrolIn combusting hydrocarbons we unlock the energy for utilization, but we also release the carbon to the atmosphere. However, nature teaches us that with an appropriate persistent energy source, e.g. solar irradiation, it is possible to effectively reverse the combustion process and “reenergize” CO2 and H2O back into hydrocarbon form."

Jan 1, 2010

By Thomas E. Weyand

Prior to 1975, lead-based paints were commonly used in protecting steel structures. Because of the toxic effects of lead on human health and the environment, their use has been significantly reduced. However, problems with these paints persist when they are removed during normal maintenance by pneumatic blasting with mineral abrasives. Technologies are developed to contain the spent abrasive and paint during blasting operations. This paper reports on A study to identify beneficial reuses for the spent blasting material. Nine samples were gathered from different projects within Pennsylvania. The samples were thoroughly characterized with regard to composition, morphology, and EP and TCLP leach test performance. Potential reuse applications will be reviewed with regard to technical adequacy, economics, and environmental constraints.

Jan 1, 1992

By Mingchun Lu, Zhe Wang, Mingming Cao, Xiangdong Xing, Shan Ren, Jianliang Zhang, Zhengjian Liu

"The effect of reduction temperature on the vanadium titano-magnetite carbon composite pellets was investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM), and the discussion has put emphasis upon the enhanced reduction mechanism of additives containing CaF2 and NaF in this paper. The results showed that the reduction temperature of 1350°C was needed for the generation, mergence and growing up of metallic iron as well as monomer dissociation between metallic iron particles and slag phase in the vanadium titano-magnetite metallization pellets. The iron compound was completely reduced into metal iron, and Fe2Ti04 was mainly transformed into metal iron, (Fe,Mg)Ti205 and FeTi03 at 1350°C. The maximum metallization ratio was only 88.5% at 13500 for 30 min without any additive. However, with the addition of 3.0% CaF2 or NaF, the metallization degree of pellets could reach up to 94.8% and 92.5%, respectively.IntroductionVanadium titano-magnetite which is mainly distributed in the area of Panxi, Chengde and Maanshan in China is a kind of complex iron ore which contains various valuable metal elements such as iron, vanadium, titanium, etc. Among the above areas, Panzhihua (Sichuan Province in China) area possesses the largest deposits of vanadium titano-magnetite and the future reserves are more than 100x108t, and the reserves of Ti existing as Ti02 reach to 8.7x108t which occupy over 91% of the whole nation and ranked No.1 in the world[1]. Lots of researches on the comprehensive utilization of vanadium titano-magnetite have been conducted in the world. And many technological processes have been applied successfully in industrial production. Among these processes, the process of rotary kiln-electric furnace is employed to recover iron and vanadium in South-Africa, while the process of blast furnace-rotary furnace is widely used in Russia and China. Besides, many researchers have made efforts on employing new direct reduction process to realize the effective comprehensive utilization of vanadium titano-magnetite[2-4]. However, the direct reduction process is only researched in laboratory and it has not been used in industry."

Jan 1, 2013

By Fathi Habashi

The recovery of uranium from wet process phosphoric acid was applied on industrial scale in the 1940's by using octylpyrophosphoric acid as an extractant. Later, more efficient reagents were used, e.g., di(2-ethylhexyl) phosphoric acid and actylphenyl phosphoric acid. In the 1970's the rare earths in Kola phosphate were recovered in Finland and recently (1997) in Norway using HNO, as a leaching agent and di(2-ethylhexyl) phosphoric acid as solvent. It was demonstrated later on laboratory scale that both uranium and rare earths could be extracted from the rock by tributyl phosphate but at different pH values provided that the rock is leached with nitric or hydrochloric acids instead of the commonly used sulfuric. This new concept opens the way to the possibility of treating phosphate rock by in-situ, dump, or vat leaching for the recovery of phosphate values as well as uranium and the rare earths. Another solvent extraction process is used industrially for the purification of phosphoric acid using butyl and amyl alcohols.

Jan 1, 1998

By Marcos Aurélio S. Costa, Nilton F. Nagem, Andreia B. Henriques, Herman S. Mansur, Alexandra A. P. Mansur, Antonio E. C. Peres, Valeria G. Silva

The superfine material generated in the Bayer process was used in one innovatively way as a precursor to geopolymerization techniques because of the presence of Gibbsite. Gibbsite can play a role in system adjustment because of the SiO2/Al2O3 ratio. Furthermore in the geopolymeric system it was studied the influenceof the additives such as kaolin, metakaolin and sodium trisilicate in an alkaline media. Others conditions to form the geopolymer were also evaluated such as solid/liquid ratio, SiO2/Al2O3 ratio and total alkaline. The raw materials and geopolymeric products were characterized by several techniques e.g. XRD, DSC, FTIR and SEM. Through the FTIR technique it was observed an increase in intensity and bandwidth in the region centered at 1010 cm-1, which is related to the asymmetric vibration Si(Al)-O, this is an indicating of the possible geopolymer formation This broadening of the band promotes a relative disappearance (overlapping) peaks at 965 and 935 cm-1 associated with raw material (ESPDust).

Jan 1, 2015

By Merete Tangstad, Fei Li

This paper studies the quartz and carbon black pellets at elevated temperature with varying temperature and gas atmosphere. High-purity quartz and commercial ultra-pure carbon black was mixed (carbon content wt.15%), and then pelletized into particles of 1-3mm in diameter. The stoichiometric analysis of the pellet during heating is studied in thermogravimetric analysis (TGA) furnace at different temperature in CO and Ar atmosphere. The microstructure, phase changes and element content of sample before/after heating is characterized by X-ray diffraction, scanning electron microscope, X-ray fluorescence and LECO analyzer. The reaction process can be divided into two stages. Higher temperature and argon atmosphere are the positive parameters for SiC formation.

Jan 1, 2016

By Bhagyadhar Bhoi, Chitta Ranjan Mishra, Hara Prasanna Mishra

"In the Sukinda Valley of Orissa, India, the total quantity of nickel ore reserves comprising of both lateritic and chromite over burden(COB) have been estimated at around 231 million tonnes containing 0.3 to 0.9% Ni. While mining of one tonne of Chromite ore, around 6-7 tonnes of chromite over burden are removed. These overburden materials are disposed as waste materials, which causes lot of environmental hazards and ecological imbalance. India imports a large amount of nickel and ferro-nickel to meet its growing demands in various sectors. For import substitutions, efforts have been made to produced ferro-nickel from the lean deposits of nickel bearing lateritic ores/ chromite over burden materials by reduction roasting followed by magnetic separation and then the nickel rich magnetic fraction is smelted to produce ferro-nickel. It has been possible to produce ferro-nickel of grade varying from 4-25% nickel.IntroductionDuring mining of chromite ore, large quantities of overburden materials are being generated. The materials amount to approximately 10 million tones per year contain around 0.3-0.9% Ni, 0.02-0.06% Co, 20-50% Fe and 4-9% Cr2O3 depending upon the location and the depth of the mine. These materials presently do not find any application for the extraction of nickel due to lack of a suitable technology. The materials are also unsuitable for ferro-nickel making because of their very high iron to nickel ratio. The country is seriously looking for a suitable technology to utilize these resources as its entire domestic requirements of nickel is met though imports. In this connection, a systematic approach has been made at the Institute of Minerals and Materials Technology, Bhubaneswar to develop a process for ferro-nickel making from this indigenous resource."

Jan 1, 2011

By Stephen Gale, David Clarry, Edmund Smith, Jon Feldman

"In 2006, a Canadian steel maker embarked on an ambitious initiative to become “Best in Class in Energy Management”. This initiative provides the framework for this paper, with some augmentation from other energy management projects carried out by Hatch. The initiative focused on identifying energy/GHG management improvements leading to low-cost implementation of energy savings or GHG emission reduction. The key components of the approach were:• Review site energy management practices and benchmark internationally.• Review best technical practices and benchmark against public energy intensity data.• Conducted a site-wide Energy Assessment and physical review of operating areas.• Facilitation of on site-workshops with staff to prioritize savings opportunities, as well as identify and remove implementation barriers.• Development of an Energy Management Action Plan for implementation of improvements.Most organizations can produce, with relative ease, a list of ideas for saving energy, implementing them is the challenge. This paper addresses these issues as well as the profitability of the energy efficiency improvements and the consequences for GHG emissions.IntroductionWhen one of the authors was an undergraduate engineering student at the University of Cape Town in South Africa, the technical drawing instructor made a statement that was both humorous, and mildly profound. He claimed that the most successful engineer is one who is both lazy and diligent. Lazy, in the sense that the engineer is constantly on the lookout for an easier, more efficient, way to do something. Diligent, in the sense that the engineer will work tirelessly to come up with a good technical solution for the easier way. This paper, somewhat of an anomaly in a compilation of technical proceedings, hopes to break the mould a little, and to show a “lazy-diligent” way of reducing the carbon emissions from an industrial facility, using a steel plant as an example."

Jan 1, 2008

By M. M. Monte

A method for removing metallic mercury from contaminated tailing, using the flotation process, is described. In order to define some relevant parameters for the mercury flotation system, microflotation and electrophoretic mobility tests were carried out on (pure) metallic mercury in the presence of several surfactants. Based on the results obtained from fundamental studies a series of bench scale flotation experiments with mercury containing tailings from two wetland sites in Brasil were done. The results of microflotation tests with mercury showed that by using cetyl trimethyl ammonium bromide, an increase in mercury flotability is observed in the acid pH range, whereas in the presence of potassium oleate the highest mercury flotability was found in the alkaline pH region. The mercury flotability using potassium amyl xanthate was improved by the addition at sodium dithionate as an activator. The bench scale flotation tests with contaminated tailings from Poconé (brazilian wetland site) showed a recovery of 70% when sodium dithionate was used as activator and potassium amyl xanthate as collector. The resulting coefficient of separation is around 60%. However, the results of the flotation experiments with fine fractions from amalgamation tailings from Peixoto de Azevedo (brazilian wetland site) showed a low mercury recovery (32%).The results from this work suggest that since in the Poconé site tailings, the metallic mercury is not completely associated to the finer particles, the flotation process to recover the metallic mercury seems very promisor.

Jan 1, 1996

By A. K. Kyllo

A study has been carried out on the dusts from Hudson Bay Mining and Smelting's Flin Flon copper smelter. The aim of the work was to determine the mechanisms of dust formation and the deportment of the various constituents. The work concentrated on the copper converters, but the electrostatic precipitators and baghouse also clean the reverberatory furnace off gas, so some mixing will have occurred. The dust composition was found to vary with distance from the furnace, and to be made up of three major components: solidified droplets, unreacted flux, and condensed particles. The solidified droplets were formed from material ejected from the converter during blowing, while the flux was blown out of the converters immediately after charging. The condensed particles contained the majority of the lead and zinc, as well as the volatile impurities. There was also a significant soluble content of the dusts, increasing with distance from the furnace. The condensed material may be separated from the remainder by a simple washing and sizing technique.

Jan 1, 1996

By den Bulck A. Van

In Europe, 50% of the copper originates from recycling. High-Cu containing scraps are regularly rich in impurities like Fe, Ni, Sn and Pb. Many high-Cu containing scraps are fed directly into anode-furnace casting installations or furnaces with limited refining capability. The impurities levels of the anodes produced in these processes should however remain acceptable for further electro-refining. The distribution of Sn between copper and slag has been investigated for conditions relevant to copper converting. Unlike previous studies, this work focuses on the behavior of Sn relevant to fire refining conditions, which are essential for anode refineries.In this study, liquid Cu–1Sn and CuOx–FeOy–SiO2 slag, with CaO additions, were equilibrated at 1300 °C in vacuum sealed SiO2 ampoules. After metal–slag equilibration, the samples were quenched in water. The composition of the slag and Cu metal was investigated with Electron Probe X-ray Microanalysis. The distribution coefficients of Sn between slag and Cu metal were determined as a function of slag composition.

By B. R. Baldock

The converting of high-grade nickel matte for production of low-sulphur matte or nickel metal is a process which has eluded metallurgists in the past because of the limitations of conventional converting furnaces. The high temperatures required and the refractory nature of nickel oxide has prevented practical success in a process which has been known to be theoretically feasible for a long time. The Ausmelt top submerged lancing system is capable of operating under close control of the smelting conditions. High temperatures and both rapid oxidation and rapid reduction can be achieved. These features have provided the basis for successful pilot plant trials of the desulphurisation of high-grade matte from the Kalgoorlie Nickel Smelter. Sulphur level in product was lowered from 20 to 25% to as low as 0.2%, with iron levels in matte in the range of 1.0 to 3.5%. The theoretical background of matte desulphurisation is surveyed and the pilot plant operations described. The implications of the results in relation to commercial plants and possible refinery operations are summarised.

Jan 1, 1993

By P. R. Taylor

Laboratory experiments have been performed to evaluate the kinetics of roasting pyrite and arsenopyrite in air at elevated temperatures, in the presence of lime. The effects of temperature, time, air flow rate, particle size, lime type, and mineral/lime weight ratio on the rates of oxidation, lime sulfation, and lime arsenation were studied. The reaction products were identified using chemical analysis, x-ray diffraction, SEM analysis, and optical microscopy. The results are discussed in terms of the utilization of lime to capture sulfur and arsenic during the roasting of refractory precious metal concentrates. More than 99.9% of the arsenic and 98% of the sulfur are contained when roasting pyrite and arsenopyrite with hydrated lime under typical roasting conditions.

Jan 1, 1991

By Marc Liebman

We present the results of a telephone survey of electric arc furnace (EAF) steel producers. This report characterizes the current status of EAF dust generation, treatment and disposal. It indicates the quantity generated, zinc content, other relevant constituents, and plans and trends that will impact on the quantity and characteristics of the dust generated. The survey covers EAF based steel producers in the United States and Canada. It identifies the processors currently employed, opinions about the use of these processors and services, as well as new technologies being considered.

Jan 1, 2000

By V. P. Bystrov

Vanyukov process has been developed and investigated in Russia over the last 25 years. It has been established that various kind of material could be treated in Vanyukov process. The results of the pilot plant trials as well as industrial experience are presented in this paper.

Jan 1, 1993

By J. R. Rendón

Cylinders of commercial aluminium alloy 6063 were homogenized under different conditions. The experimental results indicated that the general mechanical behaviour as related to curves of 0.2% yield strength, ultimate tensile strength and Brunnell hardness versus homogeneizing process is the same in both cases. The mechanical properties as compared to those required by plant specifications, tend to be better with increasing values of % Mg2Si in the alloy, as expected. The electron microscopy investigations revealed that in both homogeneizing processes the resulting microstructure consist of significant spheroidizing of the alpha phase (AlFeSi) and fine-needle type structure of beta phase. The alpha phase was also present in a Chinese type scripture. Furthermore, the slow cooling within the furnace resulted in the nucleation and growth of Mg2Si precipitates generally along the grain boundaries.

Jan 1, 1997

By B. Mishra, W. A. Averill

"The application of various hydrometallurgical, pyrometallurgical and electrochemical processes in the extraction, purification and production of radioactive metals as well as the use of various materials, ego metals and alloys, ceramics, polymers, etc. in the process, construction and handling equipment in the nuclear industry has generated a large stockpile of radioactively contaminated waste material and scrap metal which can not be directly discarded, recycled or considered for long-term storage due to its volume and potential hazards, without the separation of radionuclides. This paper reviews the emerging methods that have been investigated and suggested for dealing with some of these wastes and scrap material.The separation technologies studied for the recovery of radioactive components from the pyrometallurgical and electrochemical processing wastes have been discussed in details with results from some of the recent theoretical and physical modeling work as well as the data obtained from the actual waste treatment. Specific processes shall be described in terms of its advantages and limitations. These emerging separation technologies are being considered by the US Department of Energy as alternatives for dealing with the issues of environmental management [EM] and decontamination and decommissioning [D&D].IntroductionThe high temperature carbothermic or metallothermic smelting reduction methods for metal production are associated with the generation of significant quantity of waste as slags, flue dusts, sludges, residues, effluent salts etc. Certain hydrometallurgical processes also generate lots of aqueous waste due to the inherent nature of the technique. Also, the gas-based reduction processes are not applicable to many stable metal compounds, such as alumina, titania, beryllia, lanthanide and actinide oxides, etc. due to thermodynamic considerations. All these methods cause substantial environmental hazard. There is a need to develop alternative processes which have low waste or ideally a ""zero-waste"" generation.Pyrochemical processes using molten salts provide a unique opportunity for the extraction and refining of many reactive and valuable metals either directly from the beneficiated ore (aluminum, beryllium, neodymium, plutonium, uranium, etc.) or from other process effluent that contain reactive metal compounds. The processes reduce metal compounds electrolytically (A12O 3 and BeCI2) on a carbon anode or by calciothermic reduction (Po, Nd). The by-product, in the latter case, is a calcium oxide saturated halide salt. The waste-treatment to recycle the halide has to be done as a separate step or stored as a contaminated waste. A successful separation technology can provide a new insight to the waste minimization strategy for the nuclear industry."

Jan 1, 1996

By Tsembel Darjaa, Toru H. Okabe, Yoshiaki Umetsu

"With the purpose of extracting molybdenum and rhenium from molybdenum sulfide concentrate; .electrolysis of slurry, solvent extraction and ·precipitation operations were carried out. The slurry of the concentrate in 10 mass% NaCl aqueous solution was continuously circulated into a vertical type 10 stack bipolar electrolytic cell consisted of carbon electrode disks, and, the concentrate was dissolved by electrochemically generated oxidizers at 313 K. The current efficiency for molybdenum dissolution was 73 % after 10 hours electrolysis, and the leach solution was found to contain 0.2 mol/l of molybdenum and 4x10-5 mol/l rhenium. This result shows the dissolution is more than 8 times faster than that obtained using a single cell. The leach solution from electro-oxidation was then subjected to a solvent extraction for rhenium which is then recovered as sulfides. After rhenium separation, molybdenum was precipitated by pH adjustment, and solid MoO3 (H2O)x crystals, free of sulfate, were obtained from the leach solution containing large amount of so42-.IntroductionIn the past, electro-oxidation using a bipolar cell was applied for leaching molybdenite concentrate and ores at U. S. Bureau of Mines [1-3] and also at Bhabha Atomic Research Center [4]. In· these previous studies, Moebious type bipolar cells, in which electrode plates were vertically inserted into the free surface of the electrolyte, were employed and its effectiveness was demonstrated.Recently, the present authors studied on leaching of Mongolian molybdenite concentrate, and the effectiveness of leaching of the concentrate by electro-oxidation in alkaline and acidic NaCl solutions was demonstrated [5]. The leaching reaction during the process can be explained by the 18 electron transfer reaction of molybdenite (MoS2) with the oxidizers produced in-situ by electrolysis of NaCl aqueous solution. Further investigation was made with respect to various process parameters for electrooxidation such as pH, pulp density and temperature of the slurry, and the dissolution behavior of minor elements such as iron, copper, and rhenium [6]. Solubilities of molybdenum in the leach solution at, various temperatures and pH .was · studied, and feasibility of molybdenum recovery by hydrolysis of molybdenum species was demonstrated. By adjusting the pH of the leach solution, molybdenum oxides or hydroxides free from sulfate were successfully obtained from the solution containing large amount of sulfate ion. Rhenium present in the concentrate at a level of several tens of mass ppm was found to dissolve into the leach solution, and co-precipitate with the molybdenum compounds. Rhenium in the leach solutions, therefore, has to be recovered before precipitation of molybdenum, otherwise it is lost in the precipitate."

Jan 1, 2000

By Kensuke Sassa, Shigeo Asai, Norihisa Waki

"A new method for separating inclusions from a molten metal using a high magnetic field has been proposed. The principle of this method based on the magnetization force has been confirmed in experiments of separating intermetallic compounds imitating inclusions from molten Al-Si-Mn-Fe and Al-Si alloys. In order to measure a magnetic susceptibility, the Gouy's method has been so modified by using a super-conducting magnetic as to work in a high temperature up to 1473K. A theoretical expression for the magnetization force, which is indispensable to evaluate the magnetic susceptibility, has been derived. The magnetization forces acting on intermetallic compounds which were used in the magnetic separation were measured over the range of liquidous to solidous temperatures and the magnetic susceptibilities of the intermetallic compounds were obtained from measured magnetization forces by use of the theoretical expression.I. IntroductionRecent developments in the technology of super-conducting magnets have given rise to the circumstance that a high magnetic field over a relatively large space is readily available without liquid helium. Then, it has been found that a high magnetic field provides magnetic effects to nonmagnetic substances and various interesting phenomena have been reported in the broad science fields of physics, chemistry and biology1). ""A science related to a high magnetic field"" in which many fields are transversally viewed from the standpoint of a high magnetic field2 ) is going to be established. In particular, new phenomena and functions brought by the science related to a high magnetic field are also useful for Material Science and Engineering so that the creation of Materials Science and Engineering related to a high magnetic field"" has been conceived 3).Now, when a substance regardless of being magnetic or nonmagnetic is put in a magnetic field, it feels a magnetization force, which is familiar to such a force that a magnet attracts iron. The force is in proportion to the product of magnetic field strength, its gradient and susceptibility so that a precipitated substance can be separated from a molten metal based on the difference between susceptibilities of a substance and a melt. This is a basic principle of the magnetic separation. So far the application of the magnetic separation has been limited to the separation of ferromagnetic substances from a nonmagnetic medium. A high magnetic field, however, has enabled to separate nonmagnetic substances from a nonmagnetic medium.In this study, a new method to separate inclusions from a molten metal using a high magnetic field has been proposed. The principle of the method was verified by experimental works and the feasibility on the elimination of inclusions in steelmaking processes has been studied"

Jan 1, 2000

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