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By W. W. Albrecht

I. Introduction Refractory metals like tungsten, molybdenum, rhenium, tantalum and niobium and their compounds are essential ingredients of our modern technology. Especially in purified form, they are used in special alloys, electronics, optics and ceramics. The processing route from raw material to high purity refractory metals and their compounds includes, as a prime option, the following steps: - dissolution of raw materials. - liquid liquid extraction. - precipitation of high purity intermediate compounds. - calcination/reduction to high purity oxides/metals. Especially in the first three steps, major amounts of chemicals like acids or sodium hydroxide are used and, as by-products, substantial quantities of residues and effluents are generated. The impact of environmental regulations on these by-products and the attempt to reduce or minimize the amount of residues and effluents produced will be discussed in this presentation using Ta/Nb chemistry as the example. The basis of our considerations will be the way these by-products are handled at HCST, a major, and in some cases, the biggest producer of refractory metals (tungsten, molybdenum, rhenium, tantalum, and niobium).

Jan 1, 1992

By K. Yamaguchi, Y. Takeda

"Partial pressure - temperature - composition correlation diagrams of the Ga-As, In-As, Ga-P and In-P systems were contracted based on the obtained experimental data of the phase diagram and thermodynamic properties for the III-V systems. The total vapor pressures of arsenic or phosphorus at melting point of GaAs, InAs, GaP and InP were determined as 101, 10.1, 1510 and 253 kPa, respectively, at the corresponding melting points of 1509, 1211, 1739 and. 1336K , These diagrams are applied to the analysis of the horizontal Bridgman method and the liquid phase epitaxial growth technique. On the other hand, the analysis of the equilibrium state of the. chloride-CVD process was carried out using the data of the Gibbs energy of the compounds obtained by· authors.IntroductionThe group III-V compound semiconductors ate important materials used in optoelectronic liquid high speed electronic device. The crystal growth of the III-V compounds can involve processes that require contact between the solid, liquid and vapour phases at near equilibrium condition. Examples of processes that involve contact between the solid, liquid and vapour phases include bulk crystal growth such as the horizontal Bridgman and the liquid encapsulated Czochralski method and liquid epitaxy, and between the solid and vapor include chemical vapour deposition and molecular beam epitaxy. Therefore, the knowledge of the phase diagram and thermodynamic properties for the III-V binary alloys is essential for the analyses of crystal growth techniques of III-V compounds.For these reasons, a series of different · types calorimetric measurements had been carried out: (1) The heat contents of alloys for the Ga-As, In-As, Ga-P and In-P systems by a drop calorimeter [1;2,3]; (2) the heats of formation of the GaAs, InAs, GaP and InP compounds by a twin solution calorimeter [4]; and (3) the standard entropy of these compounds by an adiabatic calorimeter [5]. Based on the third law method, the Gibbs energies of these compounds were derived from the heat capacity, standard heat of formation and standard entropy data obtained by authors. Integral molar thermodynamic quantities of the liquid III-V .alloys were also determined from combining the heat contents of alloys with standard heat of formation and standard entropy data of the compounds· by applying the thermodynamic analysis method developed by Oelsen [6]. In the present study, the thermodynamic calculations for the crystal growth processes of the III-V compound were carried out using newly experimental data of the phase diagram and thermodynamic .properties measured by authors"

Jan 1, 2000

By Itsuki Uehara, Hiroyuki T. Takeshita, Tetsuo Sakai, Nobuhiro Kuriyama, Hideaki Tanaka

"AB5 type hydrogen storage alloys (A: rare earths, B: transition metals) are extensively applied to a negative electrode of a nickel metal hydride (Ni-MH) rechargeable battery for portable electric equipments, electric vehicles, hybrid vehicles etc. Performance of a hydrogen storage alloy electrode is affected by various factors, microstructure and surface composition of the alloy and structure of the electrode as well as composition of the alloy. Control of those factors enables us to commercialize the Ni-MH battery in various field.IntroductionA Nickel-metal hydride (Ni-MH) battery has been extensively developed because of (1) good compatibility with a nickel cadmium (Ni-Cd) battery, (2) high energy density (1.5-2 times higher per unit volume than a Ni-Cd battery) and high dischargeability, and (3) low environmental pollution. The charge/ discharge reactions can be written as [l, 2,3]:(+) Ni(OH)2+OH- = NiOOH+H2O+e· (E=+0.490V NHE),(-) l/6LaNi5+H2O+e-· = 1/6LaNi5H6+OH- (E=-0.828V NHE),where E° is a standard potential of an electrode vs. normal hydrogen electrode (NHE). Because of the above advantages of a Ni-MH battery, the battery have been widely used as a power source of portable computers, cellular phones, electric vehicles (Toyota ""LAV4L EV"", Honda ""EV Plus"" etc.) etc. Some hybride vehicles (Toyota ""Prius"" and Honda ""INSIGHT"") and fuel cell vhehicles (Toyota ""FCEV"") are power-assisted by a high-power Ni-MH battery. In 1999, the production of Ni-MH batteries reached 870 million cells in Japan. Most of commercialized NiMH batteries are incorporated with rare-earth-based AB5-type hydrogen storage alloy as a negative_ electrode. The production of rare-earth-based alloy is estimated to be approximately 8000 tons.The battery performances of the Ni-MH battery, for example, capacity, durability (cycle life), dischargeability (kinetics) and selfdischarge, ate closely related to the metal hydride· (MH) electrode, especially, the hydrogen storage alloy in the electrode. Substitution of alloy components, heat treatment, and surface treatment in order to change surface and bulk structure of hydrogen storage alloys have been examined by us and many reseachers in order to improve the performances of MH electrodes. This paper is a review of our and their efforts to improve performances of MH electrodes."

Jan 1, 2000

By Ramiro Escudero G.

Since the introduction of column flotation almost forty years ago the column technology has grown into several non-mineral applications such as among others the effluent treatment, soils recovery and de-inking of recycled paper. Recent studies have demonstrated that particular characteristics of the dispersion (bubble size, gas holdup, bubble surface area flux) are needed for a given flotation column duty. In this work, two kind of spargers were tested (i.e., internal and external) using a 4 inch column lab in a two phase system. Results show that the external sparger provides a dispersion with characteristics that include those produced by the two internal spargers.

Jan 1, 2003

By C. W. Whitten

Solis from an abandoned Pb battery processing facility were characterized prior to the selection of the extraction technique. Reflected light microscopy and electron beam methods were used to locate Pb-bearing phases and to quantify the compositions of the phases. It was found that the soils are composed primarily of quartz and feldspars with minor amounts of iron and titanium oxides. Lead is primarily present as an oxide or sulfate that is associated with the silicate minerals. Specific phases identified were PbO; Pb02; cerrusite, PbCO3; angleslte, PbSO4; galena, PbS; and magnetoplumbite, 2PbO3Fe2O3; or plumboferrite PbO2Fe2O3?

Jan 1, 1989

By Yuanbo Zhang, Qian Li, Helei Zhang, Heng Yu, Guanghui Li, Tao Jiang

"Large reserves of specularite iron ores have been found all over the world, which is characterized by high total iron grade, low gangues content, as well as low commercial price. However, it has not been widely used in sinter or pellet production due to its inferior sintering and roasting behaviors. It has shown that the proportion of specularite ores was increased as high as 40%~50% and good results was achieveed by using Composite Agglomeration Process (CAP), an innovative agglomeration process invented by Central South University. But the mineralization of specularite is still unknown during composite agglomeration processing. In this paper, the induration characteristic of specularite ore is studied by simulating CAP in laboratory, as well as microstructure analysis of CAP product. The results show that specularite pellet is mainly indurated through recrystallization of Fe2O3, calcium ferrite within high basicity sinters matrix interweaves with the recrystallized Fe2O3 on the surface of the pellet, which forms an integral microstructure, and ensures high strength of CAP product for ironmaking.IntroductionLarge reserves of specularite iron ores have been found all over the world, especially in Minas Gerais of Brazil, Xuanhua city and Anshan city of China, Elba island of Italy, St.Gotthard of Switzerland, Cumberland of Britannic, and so on. The specularite ores have a smooth surface, as well as a good crystallization and dense texture. When specularite is used to produce pellets, the specularite ore grains are difficult to adhere onto green ball due to its poor ballability. Moreover, specularite pellet requires high roasting temperature over 1300°C [1]. When specularite ore is used in sintering, the permeability of sintering bed gets bad and the quality of sinter is diminished. The practice in a few sintering plants finds that the output and strength of sinter decrease with the increase of specularite proportion, and the consumption of coke increases [2-4]. Therefore, the utilization of specularite has been limited. Composite Agglomeration Process (CAP) is an innovative technology invented by Central South University [5-7]. The process has the following merits: making reasonable utilization of different iron ore resources; improving the quality and output of sinters; manufacturing sinters with low basicity; significantly reducing energy consumption, etc[8-9]. It has been shown that large proportion specularite ores, as high as 40%~50% can be used well by CAP [10], but the mineralization of specularite pellet is still unknown during composite agglomeration processing. In this investigation, the induration characteristics of specularite ore pellets is studied by simulating CAP in laboratory, and the phase composition and microstructure of CAP product are also characterized by using microscope and Leica image analyzer (Germany, Leica DM RXp)."

Jan 1, 2011

By D. I. Davidov, D. A. Shishkin, M. B. Rigmant, E. P. Romanov, N. N. Stepanova, N. V. Kazantseva

The Co-19 at.%Al-6 at.%W alloy was prepared by two methods of casting. We used arc melting under an argon atmosphere with casting into a copper water-cooled casting mold and induction melting furnace with casting into a ceramic Al2O3 mold. According to the X-ray and SEM analyses, phase compositions depend on the cooling rate of the ingot after melting. After arc melting, the cast alloy has a three-phase structure, consisting of  cobalt (FCC), intermetallic phases CoAl (B2) type, and Co3W (DO19) type. After the induction melting, the alloy has a three-phase structure, consisting of  cobalt (FCC), intermetallic phases CoAl (B2) type, and Co7W6 () type. All phases in the investigated ternary alloy at the room temperature are ferromagnetic. Curie temperatures of all obtained phases were defined. It is shown that the magnetic properties of the studied alloy are typical for soft magnetic materials.

Jan 1, 2015

By Barry J. Welch

The production of primary aluminium can potentially lead to metal that, with minimum treatment, meets a high purity standard. Smelters that can achieve a significant proportion of their production in this manner have a competitive edge which is of growing importance as the use grows for such items as compact discs and the like. Superimposed on the desire to produce high quality metal are stringent environmental requirements that the industry must adhere to. The environmental 'legislation focuses on fluoride emissions and the approach adopted is towards a zero waste management philosophy. The fluoride recycling process does, however, result in volatile impurities being captured and recycled to the cell. Aluminium has an extremely high reduction potential and this results in a significant proportion of the recycled impurities being reduced at the electrolyte metal interface and thus contaminating the metal. This paper reviews sources of impurities and the impact of the operating procedures adopted on metal treatment.

Jan 1, 1996

By Marcelo Mourao, Adolfo Pillihuaman, Alberto Nogueira, Cyro Takano

"The self-reduction is an alternative and promising process for production of pig iron because offers decisive benefits such as enhancing the reaction kinetic with decrease in fuel consumption and C02 emissions. The self-reduction mixture of iron ore fines, carbonaceous reducer and additives for slag forming components, without agglomeration, was tested in a laboratory rotary kiln. The additives for slag were defined for presenting two different estimated liquidus temperatures (1623 Kand 1773 K) to verify the effect of these temperatures on the iron-carbon nuggets coalescence process. These mixtures were tested at 1673 and 1773 Kin an experimental rotary kiln. After reduction-melting and coalescence processes the samples were disaggregated and the iron nuggets were classified by size. It was considered that nuggets larger than 7,93mm would be a good reference for coalescence index. Low liquidus temperature slag presented 37% of this larger fraction against only 13.5% for high liquidus temperature one. The low liquidus temperature slag would facilitate contact between the particles of iron-carbon in a rotary kiln, enhancing the coalescence.IntroductionThe slag composition usually depends on the reducer ash composition, the ore gangue, the binder composition and any fluxing material [l], and the mechanism of carbon transportation in slag that contains iron oxide reducible by carbon can be explained by the oxide reduction and the metal carburization. During carbon transportation, the carburized particle is transported to slag-metal interphases by the gravity effect, being assimilated by the metallic phase [2]. When the slag's iron oxide comes in contact with the solid carbon, it is immediately reduced, forming Fe particles and CO bubbles as it is shown in the figure l(a). The Fe particles are carburized by carbon particles; they are liquefied simultaneously in the carbon-slag interphase. The Fe-C liquid particles are transported from the slag-carbon interphase to iron-slag interphase as a result of slag flow, based on the surface tension difference (Marangoni effect), figure l(b). The Fe-C liquid particles coalesce on the iron surface and the carbon is immediately diffused in the iron as it is shown in figure l(c). The reduced iron is carburized continuously by repeated sequences [3]."

Jan 1, 2013

By Patrick R. Taylor

Glass is used for immobilization of radioactive and hazardous wastes due to its durability and ability to accept a variety of waste constituents into its network structure. Alternative high temperature vitrification techniques have the advantage of increased throughput, increased waste loading and being applicable to variable and heterogeneous waste streams. However, the increased processing temperature places further concerns on the increased volatilization of contaminants, and increased corrosion and erosion of me Iter components. A database of melt properties at higher temperatures, such as partitioning, viscosity, density and electrical conductivity, in the temperature range of 1400-20000 K are being developed.

Jan 1, 2000

By T. Johnson, B. Q. Li

"Electromagnetic stirring has found a wide application in metals processing for the benefit of obtaining refined solidification microstructures. This paper presents an experimental study on the melt flow and turbulent behavior in an electromagnetically stirred Woods metal pool. The experimental setup consists of metal bath unit equipped with temperature control to allow both cooling and heating, velocity probe positioning unit and data and signal acquisition and processing unit. The whole measuring system is under the control of an IBM personal computer. Velocity measurements are made using the incorporated magnet probes, which are calibrated using a turntable. The measured results showing the effect of the coil positions, coil arrangements and the applied currents on the melt flow are presented. Both mean flow and turbulence quantities are discussed.1. IntroductionElectromagnetic stirring is widely practiced in the metals industry for melt mixing and for casting microstructure refinement. Industrial examples are taken from induction furnaces where the electromagnetic forces are applied to generate desired melt mixing and also various types of electromagnetic stirrers used in various stages of steel and/or aluminum casting processes to produce fine grain solidification microstructure or to eliminate undesired defects such as TCG (twinned-columnar-grain) structure. For ultrahigh purity aluminum or high strength aluminum alloys containing zirconium or lithium, grain refinement can be difficult with the conventional technique, and electromagnetic stirring provides a particularly powerful means to obtain the refined solidification microstructure [1]. A fundamental understanding of the melt flow and the turbulence characteristics in these magnetically-driven flow systems is of significant engineering importance to both process design and product quality improvement.There exists extensive literature on the magnetically-driven melt flows in material processing systems. Nakanish. et al. [2] were perhaps among the early investigators to mathematically and physically model the magnetically-driven flow phenomena in molten metal systems. Subsequent theoretical and experimental work by Tarapore and Evans [3, 4], Szekely and Chang [5], Hunt and Moore [6] and Szekely and El-Kaddah [7] has contributed very significantly to our understanding of magnetically-driven flow in inductively stirred melts. They have developed mathematical models for the electromagnetic field and turbulent flow in induction furnace and validated the models by either laboratory experiments or direct measurements in the industrial-scale induction furnaces."

Jan 1, 1998

By Dao-Wu Yang, Ju-Lan Zeng, Li-Xian Sun, Yan Yao

"The hydration heat of the pure cement, the fly ash single-dopped cement, as well as the fly ash and fluorgypsum co-dopped cement were investigated by means of micro-calorimety with an eight-channel micro-calorimeter (TAM Air). The results showed that the hydration heat and the hydration rate could be reduced significantly by fly ash and fluorgypsum. However, the reduction was not proportional to the loading of dopant. The exothermic peak of the fly ash and fluorgypsum co-doped cement was appeared earlier than the fly ash single-doped cement. As the temperature decreased, the hydration heat and the hydration rate of the doped cement were reduced, and the exothermic peak appeared later. The effects of fly ash and fluorgypsum on the compressive strength of cement were also investigated. The results revealed that the early compressive strength of concrete made up of the co-doped cement was largely higher than that of the fly ash single-doped cement. Based on the experiment results obtained in this paper, we could conclude that fluorgypsum is a suitable additive for fly ash-doped cement.IntroductionFly ash and fluorgypsum are industrial waste. In 2008, nearly 400 million tons of fly ash has been produced by coal-burning power plants in China. And it is estimated that this number would exceed 500 million at the year of 2015. Besides, every year the fluoride salt factories in China discharge more than 100 million tons of fluorgypsum. Tremendous of fly ash and fluorgypsum occupy considerable land and contaminate air and water sources [1]. As a result, comprehensive utilization of this two industrial waste has draw great attention from all over the world.Cement is the most-used construction material on earth. But the production of cement consumes huge energy and destroys the environment. This problem might can be partly solved by applying fly ash and fluorgypsum as additive for cement [2-4]. During the last decade, some papers that focused on applying fly ash and fluorgypsum as additive for cement have been published [5, 6]. However, to the best of our knowledge, none of these papers investigated the hydration heat of the fly ash and fluorgypsum co-doped cement.The hydration of cement is an exothermic reaction, which can result in serious problem for mass concrete: The interior of the concrete could reach very high temperature as the hydration proceeded [7-9]. As a result, the great temperature difference between the interior and the outer of the concrete would exist and cause serious thermal stresses. Thus, the concrete would be destroyed by the cracks which in tum are resulted from the thermal stresses [10, 11]. The heat released by the cement hydration and the hydration rate is commonly regulated by adding mixed materials or transferring additive such as fly ash and fluorgypsum [12-14]."

Jan 1, 2011

By Defeng Zhou, N. Trubaki, Jian Meng, Fanzhi Menga, Xiaojuan Liu, Yanjie Xia

"The microstructure and the electric conductivity of (Ce0.9Nd0.1)1 xMxO2 d (M=Mo, W) solid solutions were investigated. It has been found that their conductivity containing the grain (s gi ), the grain boundary (s gb) and the total conductivity (s t ) at 300°C- 700°C can be ranked as: (Ce 0. 9Nd 0. 1 ) 0.99 W 0.01 02- d (s gi = 0.065 S.cm·1, (s gb = 0.265 S.cm·1, s t = 0.039 S.cm-1) > (Ce0.9Nd0.1)0.99Mo0.01O2- d (s gi = 0.053 S.cm·1, s gb = 0.142 S.cm·1, s t = 0.029 S.cm-1) > Ce0.9Nd0.1 s 2- d (s gi 0.045 S.cm-1, s gb = 0.091 S.cm-1, s t = 0.018 S.cm-1) measured at 700°C. The highest conductivity is obtained in (Ceo.9Ndo.1)0.99W0.01O2 d. These results indicate that (Ceo.9Nd0.1)0.99W0.01O2- d is the most promising electrolyte materials of intermediate-temperature solid oxide fuel cells among (Ce0.9Nd0.1)1-xMxO2- d. IntroductionRare-earth (e.g. La3+, Nd3+, Gd3+ and Sm3l doped ceria-based ceramic materials have been acknowledged to be attractive electrolytes for solid oxide fuel cells operating below 600°C due to their high ionic conductivity [1, 2]. In order to improve ionic conductivity of these electrolytes further, in recent reports [3-6], some aids such as Mo03 [3] etc. in a limited amount can be used which causes extremely high conductivity. For example, Zhou et al. found that with MoO3 doping, the grain boundary conductivity of Nd3+ doped CeO2- d increased notably especially at lower temperatures due to the effect of severely undersized do pants [3]. It is well known that the size of W6+ (rw6+ = 0.60 Å) is close to Mo6+ (rMo6+ = 0.62A) because of lanthanide shrinkage. Thus, rare-earth doped ceria e.g. Nd3+ doped CeO2g with WO3 in a limited amount will be probably good and even better electrolytes. However, much less information is available about these materials. Therefore, in our paper, (Ce0.9Nd0.1)0.99 1-xMxO2- d (M=Mo, W) solid solutions have been prepared and characterized. Much higher conductive electrolytes are found in the series of (Ce0.9Nd0.1)0.99 M0.01O02- d particularly (Ce0.9Nd0.1)0.99W0.01O2- d"

Jan 1, 2012

By J. Pérez

A lead smelter slag with high copper, lead, arsenic and silver contents was treated at laboratory scale for arsenic removal. The slag was first leached at atmospberic pressure with sulfuric acid and oxygen. According to arsenic contents leaching of most of the arsenic was achieved in either one or two stages, producing a lead-silver rich residue and a solution high in copper and arsenic concentrations. Alternative routes were considered to treat the resulting solution. Firstly, solvent extraction of arsenic with a mixture of TBP and 2-etbyl-bexanol was tested and extractions of over 95 percent of arsenic were achieved. Secondly, a copper arsenate precipitation treatment was done to eliminate arsenic and copper from solution.

Jan 1, 1996

By F. J. Tavera

The column flotation technology, at first developed for application in mineral dressing, has received special attention in processing of non-mineral dispersions as a result of its low cost, high efficiency and relatively simple operation. This paper presents the results from the operation of a laboratory flotation column for the separation of vegetable oil and soap from aqueous industrial effluents, The flotation system was operated under continuous countercurrent conditions without and with additions of a cationic collector. The experiments show that it is possible to separate about 80% of the organic phase in a rougher flotation stage. These results suggest that the recovery of the organic phase is highly dependant on the dispersion characteristics (i.e. bubble size, gas holdup and bubble surface area flux) and the existing an optimum bubble size from which either smaller or larger, the recovery of the organic decreases.

Jan 1, 2003

By Staia. Mariana H.

Thermochemical equilibria of the heterogeneous system Ti-N-H-CI-Fe-Cr-Mo-Ni-Mn-C were calculated by using a commercial software based on the minimization of the free energy. Equilibrium calculations were done for temperatures varying between 800" and l 100°C and an initial molar relationship between reactants, a=NJTiCI,, of 0.1 to 2. The deposition process was considered to occur at atmospheric pressure. The activities of the alloying elements of the stainless steel were considered equal to their molar fractions. It was shown that for the conditions studied the substrate is no inert with respect to the gaseous phase. The existence of liquid chlorides was predicted for temperatures between 800" and 850°C and a ratio between 0.3 and 0.9. The most important metallic chlorides which appears to be present from the calculations in appreciable quantities in the gaseous phase are iron dichloride and manganese dichloride. In the low-temperatures zone and for low initial nitrogen contents, it result that the appearance of the liquid chlorides seems that partially inhibits the production of gaseous HCI. The highest deposition process efficiency calculated is obtained at a temperature 2 900°C and a N2/TiCI, ratios 2 0.7.

Jan 1, 1995

By John E. Litz

Metal-bearing flue dusts are produced by some ferrous and non-ferrous industries. Many dusts are being or can be treated for recovery of metal values. Operating and proposed flowsheets for the most common dusts are reviewed. Advantages, disadvantages, product marketability, and cost implications are discussed for each flowsheet.

Jan 1, 1992

By Toshihide Takenaka

The management of radioactivated stainless steel from a terminated nuclear reactor will become an important subject in the near future. The separation of the elements in stainless steel should be effective to reduce the management labor. In this study, the separation of the elements in stainless steel by an electrorefining tcchnique was investigated in an aqueous solution. The electrochemical reactions of the elements in stainless steel werc studied by voltammetry and potentio-static electrolysis was carried out. A stainless steel anode was dissolved electro-chcmically with good anodic current etliciency in a chloride solution. The residue, where Ni was concentrated, was found on the anode after electrolysis. The electrodeposit in a stainless steel cathode consisted mainly of Fe and Cr and the Ni content in it was less than 0.5wt% under suitable condition. It is concluded that an electrorefining technique is effective for the separation of the elements in stainless steel.

Jan 1, 2003

By Kang-In Rhee

A series of processes to recover the gold from electronic scrap which contains initially about 200-600 ppm Au have been developed. First, mechanical beneficiation including shredding, crushing and screening was employed. Results showed that 99 percent of gold component leaves in the fraction of under 1 mm of crushed scrap and its concentration was enriched to about 800 ppm without incineration. The scrap was leached in 50% aqua regia solution and gold was dissolved completely at 60°C within 2 hours. Other valuable metals such as silver, copper, nickel and iron were also dissolved. This resulting solution was boiled to remove nitrous compounds in the leachate. Finally, a newly designed electrolyzer was tested to recover the gold metal. More than 99% of gold and silver were recovered within an hour in electrowinning process.

Jan 1, 1995

By Hidekazu Nakagawa

We investigated the anodic dissolution behavior of titanium in TMHA-Tf2N molten salt, which has a wide electrochemical window of about 5 V, in order to develop an electrodeposition method for titanium. By etching a titanium electrode in HF?HNO3?H3PO4 solution, the titanium electrode became electrochemically active, and a redox reaction was observed at around -0.15 V vs. I-/I3- in (TMHA-Tf2N)?HTf2N solution. We identified the redox reaction consists of the reduction of the proton and the oxidation of hydrogen. The diffusion coefficient of the proton in TMHA-Tf2N was calculated to be 6.9 10-8 cm2 s-1 at 50 °C from the cathodic peak current in the cyclic voltammogram. Anodic decomposition of the molten salt was not observed up to 6.0 V vs. I-/I3- on titanium electrode, while it was observed at around 2.0 V vs. I-/I3- on platinum and glassy carbon electrodes. Cathodic decomposition of the molten salt was observed at around -3.0 V on the titanium electrode, as well as on the platinum and glassy carbon electrode.

Jan 1, 2006