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By Kerri-Ann Hue, Kerry Hasapidis, Ken Babcock, Patrick O'Hagan

"Metallic nanoparticles exhibit properties that are significantly different from individual atoms or bulk materials. Their applications are diverse and have varying uses in areas such as cancer treatment, biochemical sensors, nanoelectronics, and drug delivery. For each application extensive characterization must be performed in order to probe the unique properties of these nanoparticles. In this study, ultra-high resolution mass sensors consisting of MEMs-fabricated, suspended microchannel resonators (SMRs) were used to determine the size and concentration of metallic nanoparticles. With femtogram (10- 15 g) mass resolution, ultra-high resolution mass sensors can weigh individual particles suspended in fluid, and so measure their mass, density, and size. Particle size analysis with these sensors provides excellent accuracy and resolution compared to mature technologies such as light scattering. This technique also provides quantitative information via the ability count particles.IntroductionThe unique electronic, chemical, and optical properties associated with nanoparticles vary with their size, shape, and composition[ 1-4]. These properties are attributed to increased surface area and nanosized mean free path of electrons to the particle surface. Nanoparticle colloidal solutions have been prepared and are commercially available. In recent years, noble metals such as gold, copper, and silver have been extensively researched[5-7]. In order to tailor the optical, electronic, and electrical properties of nanoparticles, size and shape must be controlled. For many applications a monodisperse colloidal solution is ideal. Methods of size characterization include Transmission Electron Microscopy (TEM), Dynamic Light Scattering (DLS), and Electrophoretic Mobility Measurements to name a few[6, 8]. Although TEM can provide shape and size distributions, sample preparation requires that samples be dried on a metal grid and cannot be analyzed in solution. DLS uses curve fitting algorithms that while useful for determining mean particle diameters are not ideal for polydisperse colloidal solutions. New technologies are therefore needed to accurately determine the particle size distributions of metallic nanoparticles."

Jan 1, 2011

By Xiang Sun, Zheng Zhang, Jiann-Yang Hwang, Zhiwei Peng

"Nickel oxide nanoparticles were synthesized using sodium dodecyl sulfate as the surfactant and urea as the hydrolyzing agent and different calcination temperatures and time were selected for preparation. Nitrogen adsorption (BET), X-ray diffraction (XRD) and scanning electron microscope (SEM) were subsequently used to characterize the prepared samples. The effect of an external electric field on hydrogen adsorption over a prepared nickel oxide was carried out. The electric filed was introduced by a piezoelectric element, which is capable of autogenously generating charges under hydrogen pressure. Increased hydrogen adsorption was obtained from this study, which indicated a stronger interaction between the adsorbent surface and hydrogen.IntroductionMetal oxide has attracted great attention for adsorption because of their wide application in catalysis [1-7], gas storage [8,9] and sensors [10,11]. However, with respect to the usage in hydrogen adsorption, few research outcomes have been reported [12,13], since there remains the difficult task of synthesizing highly porous metal oxides with unsaturated metal centers, which account for the strong interaction with hydrogen [14,15]. Nickel oxides are polar materials with an intrinsic dipole moment. The external applied electric field could further enhance the dipole moment so that the hydrogen could be more strongly adsorbed."

Jan 1, 2012

By J. J. Talja

An investigation of oxidation of various nickel concentrates was carried out using differential scanning calorimetry (DSC). The aim of this study was to determine the ignition temperature and investigate other oxidation behavior of various sulfide-based nickel concentrates. Variables in the experiments were mineralogy, particle size and partial pressure of oxygen with temperature increasing linearly at 25 K/min from 323 to 1023 K (50-750 °C). The igni¬tion temperature was determined to represent the starting point of rapid oxidation. The reac¬tion enthalpies of the concentrates were determined and the amount of heat generated up to various time were used to calculate the extent of reaction. Mineralogical changes at various stages of oxidation were also investigated. For this purpose a second set of DSC-experiments were carried out in which each experiment was interrupted at a desired temperature between 673-873 K. From these tests the weight loss of samples were determined and changes in the individual constituent of sulfide minerals were analyzed. For pentlandite-based Ni-concentrates the ignition temperature was 705-710 K (approximately 435 °C). Pyrite was the first sulfide to oxidize. Reactivity of the violarite-based concentrate was greater than those of the pentlandite-based concentrates. The stoi-chiometry of pentlandite changed before ignition because of preferential oxidation of iron. Rapid oxidation of the pentlandite mineral occurred at about 823 K (550 °C). By 900 K about 90 % of the iron in pentlandite was converted to hematite, and NiS containing some iron was formed.

Jan 1, 1994

By Hubert Bril, Priscilla Pareuil, François Bordas, Emmanuel Joussein, Jean-Claude Bollinger

"According to the legislation, valorization type, origin and characteristics of waste material, various standard procedures are available to evaluate environmental impacts. A Mn-rich slag was sampled from a metallurgical plant. After its characterization (elementary analysis and mineralogy), five standard procedures were carried out (i.e. TCLP, EN 12457-1). Each fixed parameter of the standards was systematically studied in a large range: pH, Liquid/Solid ratio, contact time. For example, EN 12457-1 led to a low ME mobilization, increasing with the L/S ratio, the contact time and an acidic pH. As a conclusion, the representativeness of the considered parameters and their potential variations are predominant to assess of the real environmental impact during slag reuse. Introduction Recent studies have been carried out about environmental impacts of waste containing metallic elements (ME) because of their potential mobility [1-7]. Indeed, slags are either dumped or valorized in various activities such as building materials. In order to assess environmental risk, various standard procedures are used depending on country legislation, origin of waste and valorization way. Results of leaching tests are linked either to special legislation (e.g. Dumping: EC, Council Decision 2003/33/EC, Construction products: EC, Council Directive 89/106/EEC) or to legal levels used in drinking water (Directive 98/83/CE) when leachates could migrate to groundwater. If ME in leachates are lower than drinking water authorized levels, the waste will be considered as non-hazardous. On the contrary, if the leachable amounts exceed them, the question about the risk has to be posed. Beyond the abundance of leaching tests available, variety of operational conditions induced by these regulatory tests does not make the choice easier. According to operational conditions induced, ME release could vary from one test to another one. ME concentrations in leachates depend on pH, Liquid/Solid ratio, contact time and particle size [3]. To highlight the importance of these operational parameters, potential risk for valorization of a manganese-rich slag was assessed by comparing several standard leaching protocols [8-12] with a global study dealing with the influence of operational conditions. For each regulatory protocol, the most influential parameters (L/S ratio, pH, particle size and contact time) have been studied in a large range."

Jan 1, 2008

By Asmo Vartiainen

The viscosity of liquid Fe-O-SiO2 -slag at copper smelting conditions was investigated using a rotational viscometer. The studied parameters were oxygen partial pressure (10" °-10"6 bar ); composition of slag (Fe/SiO2 ratio), and temperature (1250-1400°C). The viscosity values are presented as a function of Fe/SiO2 ratio and as isoviscosity curves in ternary FeO-Fe2O3-SiO2 diagrams. The increase in viscosity at high silica contents can be accounted for the polymerisation effect of SiO4/4- -anions. At high ferric iron contents, higher oxygen partial pressure, the viscosity values increase especially near the magnetite saturation. The viscosity values are highest at the double saturation of silica and magnetite. At lower silica and ferric iron contents the viscosity values are more uniform in the homogenous liquid slag area. The viscosity values were lowest at high temperatures and highest at low temperatures.

Jan 1, 1998

By Reed M. Izatt

SuperLig® materials are capable of individually separating Rh, Pd, and/or Pt in highly purified form (99.95 to 99.99%) from a variety of chloride-based feed streams in a single stage operation. The hydrophillicity and associated kinetics of the supported materials allow for operation at relatively high flow rates of both loading and elution in a packed bed format. Pilot and commercial systems have been operated with Rh, Pd, and/or Pt present in the feed from single digit ppm (mg/l) to tens of g/l. A dual SuperLig® system for one pass Au(CN)2- separation followed by Cu and CN- recovery for CN- recycle has also been tested up to a pilot level,

Jan 1, 1999

By Tetsuya Uda

Our recent achievements of rare earth separation technique[1,2] and new process idea for rare earth magnet recycling[3] are reviewed, (1) Binary chloride mixtures of rare earths were separated by a new selective reduction-vacuum distillation process. According to our experimental results, apparent separation factors were 8.1 for the Pr-Nd chloride mixture and 570 for the Nd-Sm chloride mixture. These values are much higher than conventional solvent extraction methods. (2) A study of recycling process of magnet sludge was carried out. The rare earths in the neodymium magnet sludge were extracted by chlorination with FeCI2, An activated carbon was used as a de-oxidation reagent Metallic iron in the sludge was not chlorinated because the iron monochloride is not stable, The extracted rare earth chlorides were easily separated from Fe-alloy and the excess of FeCh by vacuum distillation, 96 % of neodymium and 94 % of dysprosium in the sludge were extraeted into chloride phase, By the vacuum distillation, a mixture of neodymium and dysprosium trichlorides of 99.2 % purity was recovered, On the other hand, the rare earth chlorides can be converted to the corresponding oxides by a pyrohydrolysis reaction accompanied by a formation of HCl gas, The HCI gas can chlorinate metallic iron to FeCh, Therefore, a new recycling process for rare earth magnet waste can be realized as a chlorine circulation type process. During the process, only carbon and water are consumed and there are no toxic pollutants, Moreover, the obtained rare earth oxide can be directly used as raw material in the conventional oxide electrolysis process,

Jan 1, 2003

By R. N. Reddy

The Pseudo capacitance of layered type Mn02 electrode material for electrochemical capacitors (EC's) was investigated. MnO2 was synthesized in our laboratory. Mn02 was prepared from heating of KMn04 at 300°C in air. Cyclic Voltammetry (CV) experiments were carried out using three electrode system, Saturated calomel electrode as reference electrode, platinum mesh as a counter electrode, and MnOz composite material mounted in a platinum mesh used as a working electrode. Two kinds of composite working electrode materials were used, one was mixture of MnOz and 25 wt% acetylene black, while the other was MnOz, 25 wt% acetylene black and 25 wt% carbon. All the experiments were carried out at 25OC. A maximum specific capacitance of 130 Fig and 118 Fig were observed at the scan rate of 2 mV/s and 20 mV/s respectively in 1M KC1 for composite electrode made with carbon. Results obtained in this study are compared with that of other electrode materials.

Jan 1, 2002

By cheng Peng-fei, TANG Hai-yan, guo Xiao-chen, LI Jing-she, Liang Yong-cang, Zhao Baojun

The origin and evolution of non-metallic inclusions for Al-killed casing steel during EAF-LFVD- CC process were studied by industrial tracer experiments. The formations of Al2O3 and MgO·Al2O3 micro- and macro-inclusions from ladle slag were analyzed by theoretical calculations. The results show that micro-inclusions were formed during deoxidation and temperature decreasing in the process of casting, most of the macro-inclusions come from entrapped ladle and mold slags. In addition, most of the Al2O3 formed were modified into 12CaO·7Al2O3 and 3CaO·Al2O3 inclusions which are liquid at steelmaking temperature. MnS cannot be fully modified to CaS and it was only wrapped outside the alumina or calcium aluminate in the form of (Ca,Mn)S with the amount of Ca-Si wire fed during the test.

Jan 1, 2016

By Thomas Niehoff, Yin Qing, Wei Zhongling, Liu Yongguo, Zhang Deliang, Tang Le

The gold ore of Shandong Gold Mining (Xinhui) was a refractory ore, which contained multi metallic sulfides (ZnS and PbS etc.) and carbonaceous. The gold ore concentrate came into leaching process and thickener and zinc replacement to recover gold. In order to improve gold recovery, the GOLDOX™ hydrometallurgy process was studied in Shandong Gold (Xinhui) by bench scale and 6 month plant scale test supported by Linde Gas. It was shown that the process promoted the leaching kinetics and improved gold recovery. The residue grade reduced 0.22 g/t in average after oxygen was applied. This indicates an operating profit increase 850,000 yuan/a in the plant. It was setting a good example for similar gold mine plant and would promote the oxygen application in Chinese gold mining industry.

Jan 1, 2015

By A. L. D. Skury

In the synthesis of diamond, the precursor graphite must present a degree of crystallinity to assure optimum yield and quality for the transformed crystals. X-ray diffraction, SEM and TEM analyses were carried out to investigate the structural and morphologic transformations produced in natural graphite by high pressure-high temperature treatment. The present study had as its objective to characterize the morphological and structural changes suffered by a natural graphite that was subjected to high pressure and high temperature treatments in the region of diamond thermodynamic stability. The results indicate that the material that constitutes the gasket, for the deformable capsule, could act as catalyst in the graphite recrystallization process.

Jan 1, 2006

By Ehsan Khajeh

In this study, the permeabilities of Al-15.5wt%Cu and Al-19.5wt%Cu have been determined by solving the full Navier-Stokes equations on 3D geometries of interdendritic channels obtained by X-ray microtomography (XMT). The samples for XMT were sectioned from different positions in directionally solidified cylinders in order to obtain a variety of microstructures for each composition. The flow has been solved using a 2nd-order accurate Finite Volume Method (FVM) approach. The effect of employing uniform or unstructured mesh on the calculated permeability has been studied. The Marching-cube triangulation method was necessary to extract accurate surfaces for unstructured volume meshing. Calculated values of permeability for this range of solid fractions show partial agreement with previous experiments. Observed deviations are attributed to the difficulties of experimental permeability measurements.

Jan 1, 2009

By P. R. Taylor

Diamond films have been successfully formed in an inductively coupled plasma (ICP) chemical vapor deposition (CVD) system from several gas mixtures: CH,-H,, C2112-112, and C2112-112-02' Our previous thermodynamic study indicated that the substrate temperature could be lowered by the presence of oxygen species at moderate system pressures (0.3-0.5 atm) and that higher volumetric growth rates required a high temperature source and a moderate pressure system in CVD processing. The principal experimental results were consistent with the thermodynamic predictions. The deposited films were characterized by laser Raman spectroscopy, scanning electron microscopy, and X-ray diffraction. The films were well faceted and uniform, with the growth rates over 10 pm/hr on molybdenum substrates. The crystal size ranged between 1 and 2 microns for a two hour experiment. It was possible to decrease the substrate temperature to below 800 °C in this system.

Jan 1, 1995

By E. Maziar Sauber

In order to prepare a more desirable feedstock for a rare earth elements separation refinery, cerium, a penalty element in the refinery feedstock, should be removed from the mixed rare earth elements oxide or carbonate feedstock. In this study, cerium (III) to cerium (IV) oxidation by calcium hypochlorite and subsequent precipitation was used to remove cerium from a mixed rare earth elements chloride solution. A factorial design of experiments was used to determine the effect of process variables such as temperature, pH, and oxidizer addition on the oxidation of cerium (III) using synthetic solutions. Under certain test conditions, all of the cerium was successfully removed from the chloride solution, and some REE accompanied cerium and reported to the precipitate. This proposed technology can allow for low cost removal of cerium from mixed rare earth elements chlorides.

By N. Kanari

The kinetics of oxychlorination of MgO by Cl2+O2 was studied in the temperature range of 850 °C - 1025 °C, using thermogravimetric analysis. The effects of C12/02 ratio, gas velocity, temperature and partial pressure of reactive gases on the reaction rate were investigated. The oxychlorination process was characterized by an apparent activation energy of about 214 kJ/mol. The reaction orders with respect to C12+O2. C12 and O2 at 950 °C were about 0.65.0.98, and -0.37, respectively. Some data about oxychlorination kinetics of MgO, Cr2O3, and MgCr2O4 contained in chromite were compared. Efficiency of using oxychlorination for the removal of iron oxides contained in magnesia was demonstrated.

Jan 1, 1999

By Ralph H. Nafziger

The feasibility of smelting a Ni-Co-Cr-bearing laterite ore from southern Oregon was evaluated by the Bureau of Mines. The objective was to prepare a master alloy for subsequent stainless steel production. A mixture of the ore with suitable reductants and fluxes was smelted in a 50-lb-capacity single-phase ac electric furnace under sub- merged arc conditions. The smelting tests produced a metal in which most of the nickel was concentrated. High-chromium recoveries required an excess of carbon. The resulting metal alloys contain sufficient nickel for some stainless steels. Ferrochromium additions would be required to attain suitable chromium levels. This research was conducted under the Oregon Metals Initiative in cooperation with Walter B. Freeman.

Jan 1, 1993

By Ryosuke Matsuoka

Keywords: Tantalum capacitor, Scrap, Recovery, Titanium, Chlorination A recycling process for tantalum from capacitor scraps using an oxidation process followed by mechanical separation and chemical treatment was investigated. This study demonstrates that sintered tantalum electrodes inside the capacitor scraps can be mechanically collected after the oxidation of the scraps in air, and high-purity tantalum oxide powder (Ta2O5) was efficiently recovered after chemical treatment. By reducing the Ta2O5 obtained through magnesiothermic reduction, tantalum powder with 99 mass-% purity was obtained. Using the chlorination for tantalum recovery was also investigated, and the tantalum or tantalum compounds were reacted with chloride wastes such as FeClx. It was found that tantalum was effectively separated and purified when tantalum powder is reacted with FeClx at 1100 K under an argon atmosphere. This recycling process utilizing chloride scrap has now been extended to other reactive metals such as titanium.

Jan 1, 2004

By Geoffrey A. Brooks, M Akbar Rhamdhani, Md Saiful Islam

A novel electrically-enhanced metal purification using slag has been developed. This was achieved by applying DC potential between liquid metal and slag phases. The concept was demonstrated through small-scale experiments at temperatures of 1500-1600oC for the removal of boron from Si-B melt using CaO-SiO2-16wt%Al2O3. Silicon (containing B) and slag were reacted in an alumina crucible in a resistance tube furnace. A circuit was produced by immersing graphite rods into the silicon bath and the slag layer. Electrical potential differences of up to 3.5 V were applied during the reactions. The reaction rates, the opencircuit voltages and short-circuit currents (in the case when the potential was applied) were then measured and determined for various slag to silicon ratio. It has been shown from this study that both the apparent rate and the boron partition ratio were increased by a factor of approximately 1.6.

Jan 1, 2014

By Michael A. Markowitz, Alok Singh

"Molecular self-assembly of phospholipids and other amphipathic molecules offers a versatile approach to form self-organized microstructures in various morphologies. Stabilization of microstructures in specific morphologies by polymerization renders them useful for practical applications in areas ranging from controlled release technology to template mediated synthesis of metals. Our efforts are focussed on the development of polymerizable biomembranes derived from phospholipids, their properties and utility e.g., as stable templates for studying chemistry at the lipid interface. Polymerized vesicles formed from mixtures of 1,2-bis(tricosa-1 O,12-diynoyl)-sn-glycero-3-phosphocholine, 1, with corresponding lipids having phosphohydroxyethanol,2, or -hydroxypropanol,3, headgroups have been used in electroless metal plating of vesicle surface with gold utilizing selective binding of Pd(NH3)4 2 + to 2 or 3. The surface bound palladium ion served as catalyst for metalization. Metalization of polymerized vesicles constructed from charge neutral diacetylenic phosphocholine,1, did not occur using this process. The headgroup structure of the negatively charged phospholipids and the degree of vesicle polymerization had an effect on the stability of the vesicles after metalization. Vesicles formed from a mixture of 1 with polymerizable diacetylenic phosphatidic acid, nonpolymerizable 1,2- dipalmitoyl phosphohydroxyethanol or 1,2-diacyl phosphohydroxyethanol (from soy lecithin) were not stable to metalization process. The metal coating of the vesicles was examined by electron diffraction and revealed that the gold metal on vesicles was polycrystalline and face centered cubic. The results demonstrate the utility of polymerized synthetic membranes as template for easy and efficient synthesis of nanoparticles. IntroductionPhospholipids, synthetic or natural, provide a simple and straight forward route to construct membranes in a variety of morphologies due to their inherent property of selforganization in the presence of water[1]. Vesicles are closed spherical structures comprised of concentric walls made from lipid bilayers. Vesicles are morphologically simple structures with enormous technological potential. Polymerizable phospholipids prepared by incorporating a polymerizable group in the molecules demonstrate physical properties comparable to their non-polymerizable counterparts and have the added virtue of providing enhanced physical and chemical stability to the membranes[2,3]. The size, shape and properties of the organized assemblies are dependent on the lipid structure and the nature of the aqueous environment[4,5]. The headgroup geometry, surface charge density, and spatial arrangement of the phospholipids are known to affect the surface behavior of the lipid membranes, which is evident through their interaction with other molecular (hormones, antigens, antibodies etc) or lomc species. Since phospholipid headgroup structure and charge can be modified either synthetically or by chemical perturbation of the aqueous medium (e.g., pH or ionic strength), phospholipid membrane surfaces offer a potential for developing novel strategies in those areas which involve the use of molecular reactive sites. One such strategy which could be envisioned explores the use of molecularly engineered phospholipid assemblies to design and prepare template structures to regulate formation of ordered materials [6]."

Jan 1, 1994

By A. V. Tarasov

Investigations of thermodynamic properties of Cu-Ni and Cu-Ni-S systems and mattes have been conducted with the aid of a MC-1301 mass-spectrometer designed for studies-of processes of vapor formation of hardly volatile substances. The instrument comprised a combination of an evaporator of Knudsen chamber type with a mass-spectrometer for analysis of the vapor phase, In the process of studies of molten Cu-Ni-S systems and commercial-grade mattes within a temperature interval of 1400-1800 K the partial pressure of sulfur was measured by means of complete isothermal evaporation and the partial pressure of copper and nickel by comparison of ionic currents. The partial pressure values of the components above the molten Cu-Ni-S were used for calculation of activities of the respective components in the melt. The copper and nickel activity data obtained was used for assessing the amount of dissolved losses of these metals in autogenous smelting slags.

Jan 1, 2003