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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 T. T. Chen, J. E. Dutrizac

"Grooved cast Pb-Ag anodes are used by some zinc refineries to improve current efficiency. It was found that the manganese oxide scale formed on a grooved Pb-0.75% Ag anode consists mainly of MnO2, which occurs characteristically in rhythmically banded colloform structures and adheres to a layer of ""Pb02+PbS04"" that oxidized from the anode. The relatively homogeneous and nearly fracture-free morphology of the ""Pb02+PbS04"" layer suggests the relatively uniform corrosion of the anode. Deposition of the Mn oxide initially follows the contours of the anode surface, but the grooves eventually become filled with Mn oxide and gypsum. Hydrous Mn oxides and amorphous Mn oxides are believed to be also present in the manganese oxide scale. Tiny particles of PbS04 and SrS04, together with gypsum, other impurities and micro-pores, tend to concentrate in the grooves.IntroductionManganese is a common impurity in hydrometallurgical zinc processing circuits. The manganese originates from sphalerite (Zn,Fe,Mn)S and from the Mn02 added to the leaching circuit to oxidize ferrous ions [1]. Manganese in the sphalerite follows Zn through the roasting, leaching and purification processes, and is present as Mn(II) in the purified ZnS04 solution. The Mn in the added Mn02 is reduced to Mn(II) during the oxidation of the ferrous ions present in the leach solutions. In both cases, MnS04 is generated, and the MnS04 accumulates in the purified solution. In the cellhouse, Zn is plated at the cathodes to produce high quality metal. The Mn(II) is partly oxidized at the anode surface to Mn(IV), and the Mn(IV) precipitates as a scale on the surface of the anode and as a sludge on the bottom of the electrolysis cells. The presence of a thin layer of manganese oxide scale on the surface of the Pb-Ag anode can minimize the corrosion of lead and, accordingly, reduce the contamination of the electrodeposited zinc. However, a heavy manganese scale build-up can cause ""staining"" of the zinc deposits and reduced current efficiencies. Consequently, periodic anode cleaning to remove excess manganese oxide scale is carried out routinely in commercial operations."

Jan 1, 2011

By Toshiyuki Kozuka

CdTe metal composite semi-conducting material has high potential in good performance of energy conversion efficiency for solar cell and there is much room for improvement of the performance by developing a process of making a thin CdTe film. In this paper, the imposition of intense magnetic field on CdTe electro-depositing surface is proposed, which is one of the possibilities for improving the energy conversion efficiency. In the experiment, cryogen-free super-conducting magnet up to 5T was used and CdTe film was deposited electrically in -o.nv vs. SHE The electrolyte was Cd and Te ammonia alkali solution with controlled temperature in the acrylic cell of 70mm diameter. Electro-deposition behavior of CdTe has affected by the imposition of the intense magnetic field due to microscopic convection in the vicinity of the depositing surface. Electro-deposited surface of CdTe becomes smooth due to microscopic convection around the surface, and the crystallization behavior is also affected, where crystallization temperature and the grain size is changed by the imposition of intense magnetic field.

Jan 1, 2003

By Toshiyuki Kozuka

CdTe metal composite semi-conducting material has high potential in good performance of energy conversion efficiency for solar cell and there is much room for improvement of the performance by developing a process of making a thin CdTe film. In this paper, the imposition of intense magnetic field on CdTe electro-depositing surface is proposed, which is one of the possibilities for improving the energy conversion efficiency. In the experiment, cryogen-free super-conducting magnet up to 5T was used and CdTe film was deposited electrically in -0.72V vs. SHE The electrolyte was Cd and Te ammonia alkali solution with controlled temperature in the acrylic cell of 70mm diameter. Electro-deposition behavior of CdTe has affected by the imposition of the intense magnetic field due to microscopic convection in the vicinity of the depositing surface. Electro-deposited surface of CdTe becomes smooth due to microscopic convection around the surface, and the crystallization behavior is also affected, where crystallization temperature and the grain size is changed by the imposition of intense magnetic field.

Jan 1, 2003

By J. H. Lee

LG Metals Corporation started its second smelter operation at Onsan along with the existing flash smelter on January 31, 1998. Onsan smelter has been producing about 140,000 tons of copper annually from concentrates with the flash smelting line since 1979. In accordance with an increase in domestic copper demand, LG Metals Corporation decided to expand smelting and refining capacity by introducing a second smelter line using the Mitsubishi continuous process and a new tankhouse in 1995. After two years' expansion works consisting of engineering, procurement, construction and a successful commissioning test, the total smelting capacity of Onsan smelter increased to 340,000 ton of copper annually from concentrates. This paper describes the smelting facilities, operation result, problems encountered and improvements during the start-up and early operation of Onsan's new smelter

Jan 1, 1999

By Sheng-hai Yang

The electrochemical synthesis was conducted in anhydrous ethanol solvent mixed with conductive reagent when tantalum plate was used as anode and stainless steel plate as cathode. The effects of different conductive reagents (such as NH4Br, (CH3)4NCl, (C4H9)4NCl), conductive reagent concentration and the space on the cell voltage and the current density were investigated. The current efficiency of electrosynthesis was more than 95%. The electrolyte, a mixed solution was then undergone air distillation and vacuum distillation to get the final product which was characterized by Fourier Transform Infrared(FTIR) spectroscopy, Raman spectra, 1H-Neclear Magnetic Resonance(1H-NMR) spectroscopy. Carbon and hydrogen contents in the product were determined by elemental analysis instrument. Results consistently show that the product was tantalum penta-ethoxide.

Jan 1, 2006

By Guan-zhou Qiu, Shui-shi Liu, Yu-feng Guo, Tao Jiang

"The preparation of high-quality synthetic ruitle from electric furnace titanium slag was systematically investigated by activation roasting followed by acid leaching process. The results showed that impurities such as Ca and Mg in titanium slag can be effectively removed and TiO2 grade of the product was markedly improved by the process. High-quality synthetic rutile containing 88.54% TiO2, 0.42% (CaO+MgO) was obtained under the conditions that roasted with 7.5%(wt) H3PO4 at 1000 oC for 2h, followed by two-stage leaching in boiling dilute sulfuric acid for 2h. Mechanism studies showed that anosovite solid solution and silicate minerals were reacted with phosphoric acid in the roasting process. As a result, titanium components in titanium slag turned into rutile (TiO2) and impurities were transformed into acid-soluble phosphate and quartz.IntroductionWith the gradual depletion of natural rutile and the rapid development of titanium industry in China, the natural rutile reserves cannot satisfy the requirement for production of titanium pigment and titanium sponge. Ilmenite is, therefore, becoming main raw material for titanium industry. However, because of its low TiO2 grade, it generally requires preconcentration to titanium-rich material such as titanium slag or synthetic rutile [1-3].Ilmenite resources are extremely rich in Pan-xi area of China, which account for 90.54% of total ilmenite reserves in China [4]. The titanium slag produced by electric smelting of ilmenite concentrate has high contents of Ca and Mg, and is not suitable as a raw material for chloride process and titanium sponge production. Therefore, upgrading titanium slag to prepare raw material suitable for chloride process and titanium sponge production has important significance for the development of China's titanium industry."

Jan 1, 2011

By T. B. Braun

Cathode contamination is the principal factor affecting the quality of electrorefined copper. It is commonly accepted that annealability is unfavorably affected by the following elements, in decreasing order of adverse effect: tellurium, selenium, bismuth, antimony, and arsenic. Silver in cathodes has importance as it represents a nonrecoverable loss of silver to the refinery. Mechanisms for the contamination of cathodes by these elements are examined and the effect of operating variables on contamination, including anode composition, electrolyte composition, electrolyte temperature, addition agent practice, and electrolyte discard rate, are discussed.

Jan 1, 1976

By Katsutoshi Inoue

Pectic acid gel crosslinked with epichlorohydrin was found to have very high selectivity to lead(II) and iron(III) ions over zinc(II) ion compared with commercial weakly cation exchange resins containing the same carboxylic functional groups, suitable for removing small amount of impurity metal ions from waste zinc plating solutions. In order to lower the cost, new adsorption gel was prepared from orange juice residue containing pectic acid by crosslinking with epichlorohydrin, which was also found to be suitable for removing these impurities. Further, very cheap adsorption gels was prepared not only from orange but also from apple juice residues by a simple method through just saponificating pectin substances contained in these residues into pectic acid by calcium hydroxide followed by water washing and drying. These adsorption gels exhibited excellent adsorption behaviors for removing the impurity metal ions away from zinc.

Jan 1, 2003

By C. Koopman

During the production of phosphoric acid from phosphate ore and sulfuric acid, large amounts of calcium sulfate are formed, in which impurities from the feedstock are incorporated. To use the calcium sulfate in, for example, the building industry, a lower concentration of impurities is desired. Mercury, copper, lead, and cadmium were extracted from clear industrial recrystallization acid (0.8-3.9 mol/kg H3PO4, 0.2-0:5 mol/kg H2SO4) by supported solvent extraction with the extracting agent Cyanex 302 in kerosene in a transverse flow hollow fiber module. The permeability for the mercury ion was 1.4.10-6 m/s, whereas that for the copper ion was calculated to be 1.5.10 m/s. Cadmium, lead, and copper were extracted during the recrystallization of calcium sulfate hemihydrate to dihydrate, an existing step within the ,phosphoric acid production process, by solvent extraction with the same extracting agent. The concentrations of cadmium and zinc in the newly formed calcium sulfate were proven to be decreased. Unfortunately, concentrations of mercury and lead were too low for analysis.

Jan 1, 1999

By Manfred Schmidt

Realizing an invention of Professors Queneau and Schuhmann, Lurgi GmbH has developed a radically new lead smelting technology, which was demonstrated on a ?30,000 tpy scale at Berzelius Metallhiltten GmbH between 1981 and 1986. Designed to treat all grades? of lead concentrates as well as complex secondaries, the novel QSL-Process applied one bottom-blown, refractory-lined long reactor and comprises two basic steps: Continuous oxygen smelting of the green charge is followed by continuous carbothermic slag reduction. Four firm orders and a number of serious inquiries from major lead producers confirm that the QSL-technology has convinced the industry of inherent process advantages. These include low investment and operating costs, flexibility and environmental acceptance. In the fall of 1986 Cominco Ltd. decided to erect a 120,000 tpy QSL plant at the site of the Trail lead smelter. Feed materials will consist of lead concentrates and zinc leach residues. The designed QSL reactor has a total length of approx. 41 m, and working diameters of 3.74 m for the oxidation section and 3. 24 m for the reduction section .. Separate gas offtakes on both sections will enable to? reduce the sulfur dioxide gas volume, and to recover a mixed zinc-lead oxide fume. Operation of the QSL reactor will start end of September 1989. First results will be presented.

Jan 1, 1990

By Jan Yaozhong

The composition and the possible utilization of Ti bearing blast furnace from a titanomagnetite blast furnace smelter were studied. The slag contained about 20% Ti02 and trace Sc. The mineralogical analysis indicated that Ti in the slag is mainly as perovskite. By means of magnetite separation, the Ti containing phase could not be enriched. An effective hydrometallurgical approach was proposed with sulphuric acid leaching. The method proposed for processing the studied slag renders product Ti02 and SC203. Besides the recovery ofTiO2 and SC2O3' the leaching process yields fine grained residues which can used as additives for making cement.

Jan 1, 1996

By P. Blazy

A hydrometallurgical procedure for the recovery of metal from ore, particularly of copper from sulphide materials is described. In the course of this procedure, the raw material is first of all submitted to the action of an appropriate reducing system and then treated with a ferric salt solution which brings about the selective solubilisation of the elements to be recovered with respect to those constituting the pyritic phase. This procedure is investigated using two ore samples proceeding from massive sulphide deposits, presenting different chemical and mine- ralogical characteristics. The results of this investigation are compared with those obtained by a classical process employing a ferric salt solution. It appears that one solubilisation of copper takes place under particularly advantageous conditions when our procedure is used. The principal parameters affecting leaching of zinc, lead and copper are examined. The selectivity of this treatment is evaluated by following the change during the treatment in the pyritic phase.

Jan 1, 1976

By Bohumír Cech, Jirí Hanika, Václav Veselý

"PET bottles are separated and subsequently crushed into flakes. Except for PET, these flakes contain PE, PVC, paper, adhesives, beverages remainders and mineral impurities. PET itself usually is a glycol and terephthalic and isophthalic acid polymer.The suggested method consists in PET flakes crystallization at 255°C. In the meantime, volatile substances evaporate and PVC disintegrates. Formed crystalline PET is crushed into small particles and then is subject to the basic hydrolysis at an atmospheric pressure. In addition to lye solution, glycol is added in the hydrolysis. Water is eliminated by boiling, which gives rise to suspension of sodium salt of terephthalic acid and glycol. The suspension is skimmed and the filtered glycol is vacuum distilled. Pure glycol is then the distillation product.Crystals are dissolved in water and the solution is filtered, which eliminates PE and impurities. Electrodialysis removes pure terephthalic acid salt from the solution. Glycol solution is returned to the hydrolysis. Terephthalic acid is precipitated by a mineral acid. Subsequently, it is washed and dried. The filtrate is separated through electrodialysis to lye and acid. The lye gets back to the hydrolysis and the acid is used for precipitation. Terephthalic acid and glycol are products in a “polymer grade” quality. The waste is a part of washing waters, distillation residues after glycol regeneration and a filter cake after the terephthalate solution filtration."

Jan 1, 2008

By Christophe Thiébaut

Keywords: Pyrochemistry, Salts Treatment, Distillation The pyrochemical purification of metal generates spent salts. When this metal is an actinide such as plutonium, the slags cannot be discarded and are thus disposed in nuclear facility. In order to handle with these slags, the decision has been taken to reduce stored quantities. The development of a pyrochemical treatment is in progress in the CEA Valduc centre. The feed salt, typically composed of various Pu and Am species contained into monovalent or divalent chloride matrix, is first oxidized to convert the actinides into oxides. Then the chlorides are separated from the actinide oxides by vacuum distillation. Temperatures higher than 750°C for monochloride salts mixture NaCl/KCl and higher than 1100°C for divalent CaCl2 base salts, are required to produce an industrial flow of vaporization. Inactive qualification of the process for NaCl/KCl base salt has been carried out with lanthanide surrogates. Then, a pilot equipment, called distillator has been designed and built for production-scale distillation of NaCl/KCl and CaCl2 oxidized plutonium salts. Industrial flows of vaporization have been obtained with this pilot equipment : about 4 g/cm²/h for NaCl/KCl at 800?900°C and 1 Pa, and more than 1,5 g/cm²/h for CaCl2 base salts between 1000?1200°C at 0.1 Pa. The last step, now in progress, is the integration of the distillator into a glove box.

Jan 1, 2005

By Alaina B. Hanlon

Keywords: Undercooling, Convection, Dendrites, Stainless Steel, Levitation Certain Fe-Cr-Ni stainless steel alloys solidify from an undercooled melt by a two-step process in which the metastable ferrite phase forms first followed by the stable austenite phase. Recent experiments have shown that the lifetime of the metastable phase is strongly influenced by flow within the molten sample. The current research will provide insight to why flow affects the metastable phase. This new understanding will lead to the use of convection to control microstructural evolution in spray-forming of stainless steels. Simulations using a commercial computational fluid dynamics package, FIDAP, yield a range of convective flow velocities that cause mechanical damage to the dendrites which is compared to experimental results. If the convective velocities are great enough that the dendrites bend, then low angle boundaries form at the points of collision. These result in high energy sites that could serve as nuclei for the stable phase.

Jan 1, 2005

By D. J. Wang

Based on the thermodynamic arid kinectic aspects, the vaccum distillation processes for the separation and recovery of metals from wastes are analyzed. As to the separation criteria, The separation coefficient and equilibrium composition relation between vapor phase and liquid phase are the bases of recovery of metals by vacuum distillation, The vaporization rates and condensation mechanisms are also discussed. Some experimental results which deal with metals-containing wastes are described and the performances of a new kind of horizontal vacuum furnace are introduced, which demonstrate that , vacuum distillation may be a prospective technique for circulation and regeneration of some non-ferrous metals from industrial wastes.

Jan 1, 1996

By Eiji Iwamura

"Two types of diamond-like carbon (DLC) films with different microstructures were prepared by unbalanced magnetron sputtering, and the tribological properties of the nanoscaled DLC multilayer coatings consisting of alternating layers of graphitelike and amorphous-like microstructures were examined. The DLC microstructure was characterized by certain features of graphite-like clusters, in that some of them had onion-like structures. The films filled with the clusters were obtained in a condition with an incidence of high influx of energetic electrons, and the other films without apparent cluster structures were formed in a condition with ion bombardment controlled by negative bias voltage applied to substrates. Stacking each film layer-by-layer, the nanoscaled multilayered coatings showed superior tribological properties to individual single-layered films due to the combination of properties induced by the difference of microstructures.IntroductionIn various tribologiql applications, it is necessary for diamond like carbon (DLC) coatings to have adequate adhesion, significant hardness and a concomitant low friction coefficient. A number of deposition techniques and coating structures have been proposed to achieve suitable DLC properties [1-3]. However it is still difficult to obtain a satisfactory level of combination of the properties particularly desirable for engineering applications.In this study, the features of unbalanced magnetron sputtering were demonstrated with the effect of ion and electron bombardment. Two types of microstructures , namely amorphous-like and graphite-like, were prepared by changing the condition of the charged particles bombardment during deposition. Using the difference of properties induced by the microstructures, nanoscaled DLC multilayered structures were examined in an attempt to improve tribological properties."

Jan 1, 2000

By M. H. Lin, S. Kou

"Czochralski pulling has been a very widely used process for growing single crystals for electronic and optical applications. Dopant segregation can significantly degrade the quality and yield of single crystals. We have used the floating-crucible technique for segregation control in Czochralski pulling, our floating crucibles being unique in that the melt passageway is very long. As such, dopant back diffusion is suppressed, even when the cross-section of the melt passageway has to be relatively large to help the melt go through or when the pulling rate is very low. Single crystals of model materials K-doped NaN03 and Pb-doped Sn have been grown with very uniform dopant concentrations. IntroductionSingle crystals of electronic and optical materials are often doped with a small amount of impurities to develop required physical properties, e.g., P and B in Si for n-type and p-type semiconductors, respectively, and Nd in YAG lasers. Dopant segregation can result in nonuniform physical properties, thus degrading the quality and yield of the resultant crystals.Figure 1 is an illustration of the conventional Czochralski process for crystal growth. Several techniques have been developed to control dopant segregation in Czochralski pulling, including the push-pull technique (1,2), the drop-pull technique (3-7) and the floating-crucible technique (8-13). The first two techniques require precise sensing devices and feedback control systems to keep the feeding rate equal to the pulling rate. The last technique is simple since the feeding rate is automatically equal to the pulling rate."

Jan 1, 1994

By Xuewei Lv

An intelligent recognition and quantification system for the micrographs iron ore sinter was developed in the current paper. The average distribution parameters in a gray histogram of minerals by a Gaussian gray distribution model were obtained. The feature curves of the gray histogram of two minerals were achieved by combining the two density functions. The feature indexes, such as the number and position of the peaks and the valleys of two minerals in different ratios, were quantified by differentiating the distribution functions. This algorithm is able to extract the feature of the minerals adequately and accurately for recognizing the composition and phases of the minerals intelligently.

Jan 1, 2009