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By Taegong Ryu

The thermal plasma process has been applied to the preparation of nanosized tungsten carbide (WC1-x). The reduction and carburization of the vaporized chloride by methane-hydrogen mixtures produced nanosized WC1-x powder, with a small amount of WC or W2C phase. The products were characterized using XRD, carbon analyzer, and TEM. The effects of plasma torch power, the flow rate of primary plasma gas (Ar) to generate plasma flame, and the addition of secondary plasma gas (H2) on the product composition were investigated. The tungsten carbide (WC1-x) powder had a particle size less than 30 nm. The powder was treated under hydrogen atmosphere to fully carburize the WC1-x, and W2C phases to WC as well as remove excess carbon in the product. Finally, WC powder with a grain size less than 40 nm was obtained.

Jan 1, 2008

By Toru H. Okabe

As part of a systematic study on the thermodynamic properties of complex nitrides, phase equilibria of the system Li-M-N (M Mg, AI, Ga) at 900 K were investigated. An attempt to determine the thermodynamic properties of complex nitrides was made by using the galvanic cell method, which utilizes LiMgN as an electrolyte under nitrogen atmosphere. The electromotive force (Emf) of the cell at temperatures between 800 and 1100 K was measured. While the Emf of the cell at 900 K was measured to be 0.137 V, data discrepancies of ±0.03 V were found. It was difficult to determine temperature dependence of the Emf. The Gibbs energy change for the reaction, 113 Li3N (s) + 1/3 Mg3N2 (s) = LiMgN (s), at 900 K was determined to be !'J.Go, (LiMgN) = -13.2 (±2.9) kJ/mol. Using thermodynamic information on the binary nitride from literature, the standard Gibbs energy of LiMgN was derived to be !'J.Go f (LiMgN)= - 121 kJ at 900 K. The thermodynamic stability range of nitride was discussed by constructing isothermal chemical potential diagrams that provide a better understanding of the stability region of the LiMgN phase. The diagram was found to be in good agreement with the isothermal phase diagram determined by the alloy equilibration method. Although the obtained data includes large uncertainties, the results provide a better understanding of the thermodynamic stability of nitrides. The potential application of this complex nitride to nitrogen chemical sensors or a medium for controlling nitrogen potential is also shown.

Jan 1, 2003

By Toru H. Okabe

As part of a systematic study on the thermodynamic properties of complex nitrides, phase equilibria of the system Li-M-N (M Mg, AI, Ga) at 900 K were investigated. An attempt to determine the thermodynamic properties of complex nitrides was made by using the galvanic cell method, which utilizes LiMgN as an electrolyte under nitrogen atmosphere. The electromotive force (Emf) of ilie cell at temperatures between 800 and 1100 K was measured. Whilc the Emf of the cell at 900 K was measured to be 0.137 V, data discrepancies of ±0.03V were found. It was difficult to determine temperature dependence of ilie Emf. The Gibbs energy change for the reaction, 113 LbN (s) + 1/3 Mg3N2 (s) = LiMgN (s), at 900 K was determined to be tJ.Gor (LiMgN) -13.2 (±2.9) kJ/mol. Using thermodynamic information on ilie binary nitride from literature, the standard Gibbs energy of LiMgN was derived to be AGO f (LiMgN)= - 121 kJ at 900 K. The thermodynamic stability range of nitride was discussed by constructing isothermal chemical potential diagrams that provide a better understanding of ilie stability region of the LiMgN phase. The diagram was found to be in good agreement with the isoiliermal phase diagram determined by ilie alloy equilibration meiliod. Although the obtained data includes large uncertainties, the results provide a better understanding of the iliermodynamic stability of nitrides. The potential application of this complex nitride to nitrogen chemical sensors or a medium for controlling nitrogen potential is also shown.

Jan 1, 2003

By G. T. Lapidus, O. J. Solis-Marcial

"The oxidative dissolution of copper from refractory minerals, such as chalcopynte, represents a technological challenge that has occupied hydrometallurgists for more than half a century. Innumerable processes have been suggested, but the majority operates at high temperatures or employs corrosive media. The origin of this refractory nature is the formation of passivating phases of iron(III) or copper. One option is to add non-corrosive ligands that complex these metal ions, thereby facilitating their dissolution. In the present work, the effect of acetone in sulfuric acid solutions was studied. The initial experiments were on chalcopynte carbon paste electrodes using cyclic voltammetry, where greater reactivity was observed. Later, leaching tests with hydrogen peroxide, cupric sulfate and ozone and, as oxidants, were performed. High extractions were achieved in three hours at 50°C. The solid residues contained the iron in the form of Fe203 and FeOOH.IntroductionChalcopyrite is the most important mineral of polysulfide copper ores [1] and accounts for approximately 70% of the world's copper reserves [2]. Currently, the copper present in chalcopyrite is extracted mainly by pyrometallurgical processes, which generate environmental concerns because of the formation of SO2 gas and submicron particulates [3]. The development of a less aggressive hydrometallurgical process for the extraction of copper would constitute a possible solution to these problems. For that reason, studies of the dissolution behavior of chalcopyrite are of great technological importance [4], However, the proposed oxidative leaching routes for chalcopyrite, generally at high pressures and temperatures, have not been implemented on an industrial scale, because of the elevated costs required to equal the high copper extractions obtained in thermal processes. These extreme leaching conditions are required because of the refractory nature of chalcopyrite. Passivation has been used to explain this phenomenon, although researchers have disagreed on the composition of the layer, which is various have assumed to be sulfur, copper sulfides, and iron-bearing jarosites or hydroxides [5]. If the latter compounds are the cause, an alternative solution would be the use of polar organic solvents in the oxidative leach to decrease the formation of the passivating iron layer. In this work, the influence of acetone on the oxidative leaching of a chalcopyrite concentrate at room conditions is explored."

Jan 1, 2012

By Ulrich Kerney

In 1996, bath smelting technology for lead recovery from concentrates and secondary materials was introduced in Nordenham to replace the common sinter plant/shaft furnace operation. Since start-up, a continuous improvement of equipment and operation lead to a steady increase of capacity and plant availability. The decision to skip the reduction stage for slag treatment now allows the treatment of 200000 t/a feed materials with a secondary fraction of up to 70 %. The main feed source for the furnace is automotive battery recycling, which offers oxide paste and metallics to be molten under oxidizing conditions in the lance fired furnace. The lead bullion is transferred to the refinery, where copper, silver and other impurities are removed. Silver is recovered as doré quality. All loopings are recycled to the BSF. Inert feed material is collected in a so-called lead concentrate of metallurgical origin, the primary slag, which is sold. It is rather a valuable feed material for further processing than a slag The off-gas is cooled in a flux-flow system, entering then an electrostatic dust precipitator. Having passed a further washing and cooling system, SO2 is oxidized and collected and sold as concentrated sulphuric acid. The presentation will cover a review of the start-up phase, the development of significant production parameters over the last years and actual production routes and figures. A comparison of environmental data between new and old applied technology is made.

Jan 1, 2006

By John Petersen

Heap bioleaching technology has become well established for the exploitation of copper sulfide ores. Still, in many operations the rate of copper extraction is rather slow, often taking two years or more to recover 80% of the copper. Chalcocite, the most common secondary copper sulfide, leaches by a two-stage mechanism. The first stage is rapid, whereas the second stage has a high activation energy and proceeds slowly at ambient temperatures. Nonetheless, this rate is still considerably faster than what is typically realized in a full-scale heap. A comprehensive column bioleaching study of a chalcocite ore has shown that the chalcocite columns are leached in a zone-wise fashion. The first zone corresponds to the first stage of chalcocite leaching, where all ferric produced by the bacteria is immediately consumed and all acid entering with the feed solution is consumed within a relatively narrow band. The second stage of chalcocite leaching proceeds much more slowly in the wake of the first stage, within a zone that grows gradually over the entire length of the column. The overall rate of leaching is thus determined by the rate of acid supply into the column rather than by mineral or bacterial kinetics, at least until the entire column is engaged in second-stage chalcocite leaching. In full scale heaps, there is evidence to suggest that solution distribution favours channelling between relatively large clusters of material which are exposed only to stagnant solution. Reagents have to migrate into such clusters by diffusion, which retards the delivery of acid dramatically. Thus, we believe that the rate of chalcocite oxidation in heaps is governed by sideways diffusion rather than downward migration. Column experimental results have been reproduced with a comprehensive heap-modelling tool. The model predicts that by simply changing the length of the average diffusion channel from column conditions (a few cm) to heap conditions (tens of cm), extraction times can change from weeks to years under otherwise identical conditions.

Jan 1, 2003

By P. A. Metz

The Fairbanks mining district has produced in excess of 7.5 million troy ounces of placer gold and 250,000 troy ounces of lode gold since gold was discovered in the area in 1902. The Fairbanks mining district is in the northwestern part of the Yukon-Tanana Upland Schist Terrane, an area of approximately 240,000 square km that has produced in excess of 21 million troy ounces of placer gold. All lode gold production from the terrane has been from the Fairbanks mining district, and all of this production has come from high-grade gold-quartz polymetallic sulfide veins. Gold grains in the vein systems range in size from several microns to several millimeters. The veins are localized in a complex metamorphic rock assemblage which includes greenstones and felsic metavolcanic and volcaniclastic rocks, meta-exhalatives and metasediments. Gold occurs in the metamorphic host rocks in association with arsenopyrite and arsenic-antimony sulfides which occur in lenses and disseminations within the host rock. Gold grains occurring in the metamorphic host rocks range. in size from sub-micron to a few microns in diameter.

Jan 1, 1987

By Ray D. Peterson

The hydrothermal enrichment of chalcopyrite by CuSO, occurs in the absence of oxidizing or reducing reagants. Kinetics of the enrichment process were determined under autoclave conditions in the temperature range of 398°K (125°C) to 473°K (200°C). Covellite (CuS) formed first, followed by digenite (Cu,,,S), with rejection of iron to the solution. The kinetics have been explained by a model which includes diffusion during the first stage formation of covellite followed by surface reaction rate control when digenite be. The effects of particle size, temperature, pH, and cupric and ferrous ion concentrations on the leaching kinetics were examined. Additions of ferrous ion to solution markedly increased the rate of reaction.

Jan 1, 1994

By Hans Jürgen Maier, Gregory Gerstein, Florian Nürnberger

Microstructural analysis to support the development of material models provides valuable information to design complex forming operations. Damage models such as e.g. by Gurson consider spherical voids only. However, investigations of bcc steels by scanning electron microscopy reveal that voids exhibit an ellipsoidal shape with progressing deformation. The material’s weakening in the Gurson model is taken into account by the void volume fraction. Therefore, a three-dimensional characterization of the void shape offers important data for modelling. Thus, information on the anisotropy of the process of void evolution and accordingly, about the anisotropy of the deformation process is provided. Application of the information regarding the void shape anisotropy within the Gurson model is discussed.

Jan 1, 2016

By Sumantra Mandal

The hot deformed microstructure of the 15Cr-15Ni-2.2Mo-Ti modified austenitic stainless steel (commonly known as alloy D9) was investigated employing electron backscatter diffraction (EBSD). Hot compression tests were conducted in a Gleeble thermo-mechanical simulator at temperatures of 1173K-1373K (in steps of 100K) with a strain rate of 10 and 100 s-1 to different strains. Various kinds of deformation patterns were observed inside the deformed grains. These were inferred as the development of geometrically necessary boundaries or formation of parallel set of micro-bands. Recrystallized grains were partitioned from the deformed grains employing grain orientation spread approach. Extent of dynamic recrystallization (DRX) was found to be minimal at 1173K. DRX was predominantly found to happen at and above 1273K which increases with increase in strain. DRX nucleation and development mechanisms were discussed with respect to bulging of the parent grains and sub-grain rotation. Special emphasize is given on the role of annealing twins on DRX nucleation and subsequent expansion.

Jan 1, 2009

By S. P. Rivers

The stainless steel industry re1ies on nitric-hydrofluoric acid (HNO,/HF) pickling solutions to remove surface contaminants and maintain the corrosion resistance of the steel. More stringent environmental guide1ines are expected to be placed on the disposal of these solutions which could significantly increase processing costs. The U.S. Bureau of Mines has been conducting research to develop a process for recycling depleted pickling solutions, thus reducing the quantity of by product acids generated. Research has shown that F- can be liberated from the predominant iron fluoride species (FeF,') by using oxalic acid in an electrodialysis cell. Ion selective membranes allow dissolved metals in the depleted solution to be replaced with hydronium ions by metathesis, thereby regenerating the HF. The regenerated HN03/HF is then retained in the pick1ing solution. This paper reports on the research effort at the U.S. Bureau of Mines Rolla Research Center to apply electrodialytic recycling to HN03/HF pickling solutions.

Jan 1, 1993

By M. H. Staia

A Venezuelan ilmenite concentrate has been chlorinated at a temperature of 700" C by carbon tetrachloride. In the experimental rig, built at laboratory level, the direct chlorination process yielded a TiCI, recovery of approximately 85% after 280 minutes processing. The partial pressure of carbon tetrachloride was nearly atmospheric (0.94 atm). Product vapors from the reactor were fractionally condensed in a condenser which was maintained at a temperature of 250°C meanwhile TiCl, vapors were condensed in refrigerated coils at a temperature of -20°C. The concentrate used in this investigation was obtained by applying gravitational and magnetic concentration methods to the black sands. The experimental results have shown the need to asses the influence of the weight ratio of ilmenite to carbon tetrachloride on the resultant products. The equilibrium of the heterogeneous system has been calculated taking into account the initial experimental conditions.

Jan 1, 1995

By C. A. Young, J. D. Miller

Adsorption isotherms previously determined by in-situ Fourier transform infrared/internal reflection spectroscopy (FT-IR/IRS) for oleate adsorption at calcite and fluorite surfaces near pH 9 and at various temperatures are compared. Results indicate that, at both mineral surfaces, chemisorption occurs at equilibrium concentrations below approximately l x l0-5 M oleate while calcium dioleate surface precipitation occurs at higher equilibrium oleate concentrations. The extent of chemisorption at the calcite surface is 3 to 5 times less than that at the fluorite surface while the extent of calcium dioleate surface precipitation on calcite is nearly a magnitude larger than that on fluorite. However, for both minerals, surface precipitation decreases with increasing chemisorption. Contact angle measurements and flotation recoveries show the hydrophobicity of fluorite to be greater than that of calcite at each of the temperatures and oleate concentrations studied. Significant differences are noted only in the chemisorption region. Unlike calcite, the hydrophobicity of fluorite was sensitive to the presence of oxygen in the system. Multichannel Laser Raman Spectroscopy (MLRS) showed this behavior was caused by the double-bond reactivity of adjacent chemisorbed oleate molecules and subsequent formation of an epoxide/polyether complex at the fluorite surface. Such a reaction product could not be detected at the calcite surface. These differences in adsorption density, hydrophobicity, and polymerization behavior are discussed in terms of the intrinsic surface properties of the minerals.

Jan 1, 1999

By S. L. Pohlman

Physical characteristics of possible importance in the acid leaching of Chrysocolla have been evaluated. Surface area studies and pore size distribution indicate: 1) a large surface area (350 m /gm); 2) an average pore size of 13 or 16 Å , depending upon use of the adsorption, or desorption, branch of the Type IV isotherm in the evaluation; ) the presence of a significant fraction of pores of size less than 15 Å determined by the accumulation surface area method. The initial structure is micro- crystalline on the basis of x-ray powder patterns; the silica leach residue is amorphous and has only 24 m2 /gm surface area, and loses integrity when dry. However, readsorption of copper onto the wet leach residue gives a product with integrity and 100 m2 /gm surface area. Visual observation of the leach residues supports evidence of a non-protective diffusion mechanism of leaching which is well correlated by the shrinking core model previously presented.

Jan 1, 1976

By Roger Altman

The solubility of copper in primary spinel crystals encountered in reverberatory slag samples has been determined by electron microprobe analysis. These spinels, which ranged in composition from 22% A12O3 to pure magnetite, contained small quantities of dissolved copper (0-0.4%). Based on literature data it was estimated that the solubility limit of copper in solid magnetite is no greater than about 1% at 1200°C and about 2% at 1250°C. However, it was found that practically every spinel crystal examined contained significant amounts of matte inclusions. Further examination of converter slag revealed large quantities of irregularly shaped precipitated magnetite crystals which contained a large proportion of copper inclusions. Additional experimentation showed that the total copper content in reverberatory slag samples was greater than the sum of the estimated en- trained plus dissolved matte in the slag. This difference is believed to be significant and is due to the presence of matte inclusions in the spinel crystals. In the present reverberatory slag samples these inclusions accounted for about 1/2 of the amount of sulfide directly entrained in the slag.

Jan 1, 1976

By Jim Hardy, Tim McKnight

"The thermal mass flow controller, or MFC, has become an instrument of choice for the monitoring and controlling of process gas flow throughout the materials processing industry. In the semiconductor industry, these MFCs are used on over 70% of the processing tools. Reliability and accuracy are major concerns for the users of the MFCs. Calibration and characterization technologies for the development and implementation of mass flow devices are described. Sources of inaccuracy in process gas handling are described, and a model to correct for these inaccuracies is outlined. A gravimetric calibrator is described that allows flow sensors to be calibrated in corrosive, reactive gases to an accuracy of 0.3% of reading, at least an order of magnitude better than previously possible. All described capabilities are implemented in a Department of Energy User Facility which is available to industry and universities to test and develop gas flow sensors and controllers and evaluate their performance related to environmental effects, reliability, reproducibility, and accuracy.IntroductionMaterials processing is at the heart of semiconductor manufacturing. To make today's advanced integrated circuits, silicon wafers are subjected to over 200 process steps. Most of these steps involve processes such as etching, implanting, diffusion, annealing, deposition, and lithography (resist deposition and hardening). Often one or more process gases are used to complete the process step. To achieve the quality and performance required in the micro devices, accurate measurement and control of these gases is essential. The Oak Ridge National Laboratory (ORNL), in conjunction with the semiconductor industry, has been working to improve process gas measurement and control accuracy and reliability. Standardized test methods have been developed to characterize and benchmark the performance of mass flow controllers (MFCs), the method of choice for monitoring and controlling gas delivery. Testbeds have been designed and fabricated to produce repeatable and accurate data using these standards. Baseline testing was performed along with development of a unique mass flow instrument, the gravimetric calibrator."

Jan 1, 1997

By N. M. S. Balbinot, A. L. Rodríguez, C. M. Mahlmann, R. de C. de S. Schneider

The use of sunflower oil co-products it was studied for production thermoplastic composites. Thermoplastic composites have been processed in polyethylene matrices of virgin linear low density polyethylene (LLDP) or recycled. Samples have been formulated with 10% mass fraction of sunflower bran, seed coat and mixture of bran and seed coat. The material characterization has been achieved by mechanical tensile test and Shore D hardness and by density physical testing. The results have demonstrated better properties to thermoplastic composites with sunflower seed coat.

Jan 1, 2008

By Takashi Ikeda, Masafumi Maeda

"Demand for solar cells is increasing linearly throughout the world. Last year production totaled 3000 tons worldwide. The market size of solar silicon is expected to increase further because of international ""political"" demand to reduce carbonaceous emission from energy consumed. Most elemental silicon is produced by the carbon reduction of Silica in an electric arc furnace. Purity of silicon at this stage is 90-99%. Major impurities are Fe, Ti, Ca· and Al, and minor ones are P, B and carbon. The oxidizing metallurgical process is no longer effective to remove transitfon metals because those are less noble to silicon. Nonmetallic impurities such as phosphorus and boron must be reduced to 0.001ppm for semiconductor use. The most common process for high purity silicon is the Siemens C process, which is basically distillation of hydro-chlorinated silicon followed by CVD of SiHCl3. The cost of such silicon is expensive to allow its popular use in solar cells. Currently scrap silicon -of semiconductors is used for this; however, the supply-of that scrap is limited to just a portion of semiconductor production.In this paper world demand for silicon will be reviewed and some of the processes proposed summarized.IntroductionSilicon is element 14 in atomic number and has an atomic weight of 28.0855. Little elemental silicon is found in the earth, and it is mostly found as oxides or silicate. The Clark number of silicon is very large and the second in its number. If we were discussing the volatility of silicon element on the globe, we would never worry about it. However, it is very difficult to obtain pure elemental silicon because a high purity silicon compound is very rare. In most cases these are silica (silicon oxide SiO2). As shown in Table 1, there are many grades of silica ore classified mainly by their content of iron and alumina."

Jan 1, 2000

By Yoichi Takeda

Copper solubility in Si02-CaO-FeOx slag equilibrated with copper matte in 10% S02 atmosphere at 1573K was estimated. Essential parameters are activity coefficients of copper oxide and sulfide, oxygen and sulfur potentials and activity of copper in the slag-matte system. A large number of experiments provide proper parameters to calculate copper solubility in slag. A classical thermodynamic model postulating CUOO.5 and CuSo.; molecules assists in estimating copper solubility in slag. Additions of Si02 and CaO reduce copper solubility almost in any condition. Copper loss, that is function copper solubility and slag volume, in the silica saturated Si02-FeOx binary slag is minimally equilibrated with less than 66% copper matte while copper loss in the 50% FeOx-SiOrCaO ternary slag saturated with 2CaOSi02 is minimally equilibrated with over 66% copper matte. This slag composition has potential for continuous copper converting, direct copper production or high-grade matte production.

Jan 1, 2003

By Roberto Parreiras Tavares, Frederico da Costa Fernandes, Guilherme Antonio Defendi, Vangleik Ferreira da Cruz, Júlio César de Sousa Pena

"Near-net-shape casting is an important area of research in the iron and steel industry today. Among the near-net-shape casting processes, the single-belt caster seems to be the most promising, since it is the only one that can achieve levels of productivity similar to those obtained with conventional continuous casting machines. One of the most important aspects in the single-belt casting is the feeding system used to deliver liquid metal over the belt. This system determines the velocity distribution and the levels of turbulence of the liquid metal and affects the quality of the strips. In the present work, a metal delivery system having a simple geometry was proposed. Using the CFD code CFX 5.6, a mathematical model to simulate three-dimensional turbulent fluid flow and heat transfer in that system has been developed. This model was used to analyze different configurations of the metal delivery system and the free surface shape of the fluid was also determined. A physical model of the feeding system was built and used to validate the predictions of the mathematical model. The fluid flow calculations have been validated by dye injection experiments and laser doppler anemometry. Measurements of the free surface levels have also been performed. These experiments provided supporting evidence for the predictions of the mathematical model.IntroductionTo maintain its competitiveness in the present market, the metallurgical sector, particularly the steelmaking companies, are developing new techniques of production. Some of these new processes are focussed on the strip casting technologies. Among these technologies, the SingleBelt process is considered the most interesting option, reducing the number of rolling steps and, consequently, the final cost of the product, especially the part associated to the energy consumption (fuel and/or electric energy). This process can also reach levels of productivity that can not be matched by other strip casting methods(1). One of the most important aspects concerning these new processes is related to the liquid metal delivery system. This system can have a significant effect on the final quality of the strips, since it determines the velocity distribution and the levels of turbulence of the liquid metal."

Jan 1, 2004