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By H. Hahn, B. H. Kear, K. Kan, S. C. Danforth, G. Skandan, W. Chang

"A new chemical synthetic process for the production of non-agglomeratednano structured ceramic (n-ceramic) powders, starting from metalorganic precursors, is described. The process combines rapid thermal decomposition of a precursor/carrier gas stream in a hot tubular reactor with rapid condensation of the product particle species on a cold substrate. Critical to the success of this Chemical Vapor Condensation (CVC) process are (1) a low concentration of precursor compound in the carrier gas, (2) rapid expansion of the gas stream through an uniformly heated tubular reactor under a reduced inert gas pressure of 1-35 mbar, and (3) rapid quenching of the gas phase nucleated clusters or nanoparticles as they exit from the reactor tube. A wide variety of metal organic precursors is available commercially, all of which can be utilized in the CVC process to produce n-ceramic powders, including single phase, multiphase and multicomponent systems.The CVC process has been used to synthesize non-agglomerated n-SiCxNy and n-ZrOxCy powders, with controlled particle size in the range 2-20 nm. Heat treatment of the assynthesized n-powders in various high purity gas streams causes compositional and structural modifications, including particle purification and crystallization, as well as transformation to a whisker-like morphology. Thus, as-synthesized amorphous n-SiCxNy particles transform to (1) cubic n-SiC particles, when heated in flowing argon at temperatures> 1350 °C, (2) hexagonal n-Si3N4 whiskers, when heated in flowing NH3IH2 at 1400 °C, and (3) cubic nSiC whiskers, when heated in flowing H2 at 1400 °C.Non-agglomerated n-ceramic powders form uniformly dense powder compacts by cold pressing, which can be sintered to theoretical density at temperatures as low as 0.5 Tm' For example, full densification ofn-Zr02 powder compacts under free sintering conditions can be achieved at 1125 °C."

Jan 1, 1994

By R. Boom, B. Kraaijveld, H. Kuntzel, Y. Meteleva-Fischer

"Alloying refining with rare earth elements followed by acid leaching was examined for the potential of upgrading of metallurgical grade silicon. Microstructure study of silicon alloyed with small additions of rare earths showed behavior relatively similar to the influence of calcium addition. After alloying with neodymium the phosphorus content was detected in various intermetallic silicides containing neodymium and iron. The content of lanthanum and neodymium in refined silicon was by several times lower than that of aluminium and calcium. Alloying with lanthanum and neodymium at smaller additions than calcium reduced the phosphorus content down to the same level. The efficiency of lanthanum and neodymium in removal of boron and phosphorus at the 1-2 wt% of their additions and their low solubility in silicon make the alloying with these metals followed by acid leaching an attractive option for the refining route of metallurgical grade silicon up to solar grade.IntroductionA striving for a cheap ""green"" energy directs the research interests in silicon solar cells towards new efficient refining routes for metallurgical grade silicon (MG-Si, -98% purity). The silicon price determines up to high extent the solar module's price, so that cheap and efficient metallurgical process is awaited. The research challenge is to fulfil the purity requirements of solar grade silicon (SoG-Si, 6N) by competing with the energy-consuming and environmentally unfriendly Siemens process. Most difficult impurities to remove are boron and phosphorus, so technologies dedicated to their efficient removal attract an attention of industry and academia.Alloying refining (also known as solvent refining) is one of the most promising refining options, which is based on a principle of solid-liquid extraction using limited solubility of impurity elements in solid silicon [ 1]. Various elements were proposed for alloying refining: aluminium [2], calcium [3], tin [4], iron [5], copper [6] etc. The attractiveness of the alloying refining is in decreasing a melting point of the metal mixture and an affinity of the alloying element to the most harmful impurities, especially to boron and phosphorus. However, the difficulties are still faced due to self-solubility of the alloying elements, their low affinity to boron and/or phosphorus, silicon losses and necessity of removal of the silicide impurity phases in an additional step, using acid leaching [7], fractional melting [ 8] etc."

Jan 1, 2013

By Bradley C. Bockrath

Some thirty coals were evaluated for liquefaction activity under a mixture of CO and H2 at 425° C. The viscosity of the liquid products was taken as an indicator of the degree of liquefaction. It was found that the direct liquefaction of a particular coal may be beneficially influenced by the presence of pyrite. Active pyrites are often found in the native mineral matter of the coal itself. For example, subbituminous and bituminous coals and lignites of relatively high pyrite content were found to liquefy more readily than similar coals or lignites which were poor in pyrite. The reactivity of inactive coals could be improved by using blends with active, pyrite-rich coals. In addition, pyrite was effective when added separately as pyrite concentrates obtained from coal beneficiation operations. Various other iron- and sulfur-bearing additives were also effective when used in combination as added slurry-phase catalysts, including iron oxides and mineral residues derived from liquefaction of active coals. Under liquefaction conditions, pyrrhotite ( Fe I- x5) is formed from pyrite or from the iron oxides and many sulfur containing species. Pyrrhotite was shown to be a hydrogenation/dehydrogenation catalyst for tetralin but is not active for initiating a variety of free radical reactions that do occur when pyrite is heated with tetralin. The role of pyrite in coal liquefaction is complex and still not well understood.

Jan 1, 1981

By John Hanna

The University of Alabama Mineral Resources Institute (MRI) has developed a unique process for selective fatty acid flotation of carbonate gangue from sedimentary apatites (francolite) in the pH range of 4-6, without collector conditioning of the pulp. The process, which does not require an apatite depressant, was modified to beneficiate a high MgO siliceous phosphate matrix from South Florida. The modified process includes two flotation stages, one for carbonate removal, as mentioned above, and the other for phosphate recovery from the siliceous gangue. The selective flotation separation of the carbonate and phosphate from siliceous constituents of the matrix at various pH levels and collector dosages are discussed. In the carbonate flotation stage, about 70% of the MgO was rejected in the froth, and the phosphate flotation stage produced concentrates analyzing about 31% P20S' 0.7% MgO and 4% acid insolubles. The overall P20S recovery in the two stages is about 85%.

Jan 1, 1989

By A. Mezei

Samples of cobalt and bismuth concentrates produced from the NICO deposit in Northwest Territories were subjected to a comprehensive metallurgical testwork consisting of: pressure oxidation, ferric chloride leach and carbon in leach, to recover the cobalt, bismuth and gold, respectively. A specific testwork program was designed to allow for the optimization of process parameters under multiple restrictive criteria. The overall objective was to establish leaching sequences that could produce acceptable recoveries while generating environmentally disposable residues as well as solutions suitable for further processing. The recoveries for the leaching stage, under the optimum conditions, were 97% for cobalt and 95% for gold, in the case of the cobalt concentrate. The bismuth concentrate produced recoveries of 99% for bismuth, 99% for cobalt and 97% for gold, respectively

Jan 1, 1999

By Yang Jian-guang, Deng Zi-xiang, Zhang Xu-liang, Li Jun-yuan

"Hyperaccumulator biomass harvested after heavy-metal phytoremediation must be considered as hazardous waste that should be contained or treated appropriately before disposal or reuse. As a potential method to detoxify the biomass and to convert this material to a suitable bio-energy resource, the hydrothermal upgrading process was applied to remove heavy metals and upgrading crude bio-oil from Pteris vittata stems and leaves harvest. Parameters such as material granularity, temperature, Liquid/Solid (L/S, ml/g), pressure, duration and catalysts were examined for their effect on the removal efficiency of heavy metals and upgrading efficiency of crude bio-oil. Maximum heavy metal removal efficiency of>99% and crude bio-oil upgrading efficiency of 83% were attained with an 200 mesh (75 µm) granularity, LIS 40:1and23 MPa at 380°C in the presence ofO.l mol L-1 K2C03 for 30 min. GC-MS analysis results show that the resulting bio-oil mainly consists of benzene 11 %, ketone 42%, alcohols 14%, alkene 15% and ester 11 %, etc., and the relative molecular weight distribution lies in 94-282, carbon number distribution lies in 6-18, calorific value is 32MJkg-1.IntroductionPhytoremediation of soil or water with hyperaccumulator has been extensively explored in recent years [1-4]. Living plants can clean up soils or waterways. This approach exploits the ability of various plant species to thrive in high metal environments where large amounts of toxic elements are accumulated, such as heavy metals, and is particularly appropriate when slow remediation of relatively low metal concentrations is acceptable. Advantages compared with existing remediation methods include the minimal site destruction and destabilization, low environmental impact, and favourable aesthetics; advantages compared with biosorption include continuous in situ regeneration of the biomass, and the ability of living plant cells to supplement passive sorption of metals with metabolic mechanisms of metal uptake and detoxification [5-8]."

Jan 1, 2014

By Dalene Joalet Steenkamp

Excavation of industrial-scale furnaces allows for the systematic study of reaction sequences by identifying the different reaction zones within the furnace. In 2013, Transalloys excavated a 48 MVA submerged arc furnace that was used for silicomanganese production using the ore-based route. The excavation method was reported elsewhere as was observations made in terms of refractory wear and modes of electrical energy dissipation prior to excavation. The paper presented here, reports on the process reaction zones observed during the excavation and subsequent phase chemical analyses of a number of process samples obtained during the excavation. The zones identified were a loose burden zone, a dry coke-bed zone, a wet coke-bed zone, a hard build-up zone, and an alloy zone. The results are compared to observations made in the excavation of an industrial-scale SAF and a pilot-scale SAF in Norway. The presence of the hard build-up zone below one of the electrodes and absence of a slag zone below all three electrodes are unique features of the SAF excavated at Transalloys.

By F. Garcia-Carcedo

This research aimed to develop a clean technology for the production of ZnO from residues generated by the steel making industry. Scientific and technologic parameters were both investigated in order to define an industrial methodology allowing the integral recycling of EAF dusts. A reengineering of the Waelz process was perform,~d, aiming to produce a clean fraction of ZnO, fluorine free, as well as a slag enriched in metallic iron, which can be recycled in electric arc furnaces. The technical conditions used to produce the ultra pure fraction of ZnO are described. The magnetic separation of the EAF dust allowing the production of a phase high in iron and recyclable to the electric arc furnace is also discussed. Thermodynamic of the volatilization of all the elements contained in the EAF dust was performed in order to better control the thermal process in the rotary kiln. Tests were run using different reducing agents, weakly or highly reactive, aiming to determine their specific efficiency.

Jan 1, 2000

By Fei Ruan, Chang Jie, Jieyu Zhang, Jifang Xu, Kuochih Chou

"Viscosity is an important physical parameter of slag in metallurgical processes. Most studies of aluminosilicate and aluminate systems assume that aluminum occurs in tetrahedral coordination. In this case, the O/Al value was utilized to describe the slag structure in terms of the network character of aluminosilicate and aluminate systems. Composition and viscosity data from the literature and the trends were analyzed according to the O/Al value and temperature. It is shown that the O/Al value explains the trends in more than ten systems, containing more than 200 data points. In aluminosilicate system, the trend that viscosity value changed with the O/Al value which implies that alumina works as network modifier such as basic oxides or works as network former. In aluminate system, irrespective of the system and temperature, viscosity decreased steadily when O/Al value increased.IntroductionMetallurgical slags, which are made of oxides and many also contain fluorides, play an important role in metallurgical processes such as iron making, steel making and secondary refining processes. Aluminosilicate slags are applied in a wide range in metallurgical processes. A polymerizing effect of the addition of aluminum and an association of aluminum with low-field strength cations is further supported by the physical variations in aluminosilicate and aluminate systems. The behavior of alumina in silicate melts has been studied by various authors [1-6]. It is generally accepted that Al2O3 is amphoteric [7] because Al3+ ions can behave in profoundly different ways in a silicate melt. When added to a pure silica melt, Al2O3 acted as a network modifier, breaking the bridging oxygen of the pure silica network, thereby decreasing the viscosity in a similar manner to other network modifiers, such as CaO, MgO etc. to form [1/2Ca (AlO4)]4- complexes. However, when added with alkali or alkali-earth metal oxides, some of the Al3+ ions assumed tetrahedral coordination and replaced Si in the liquid network, the missing charge was compensated by Me+ or Me2+ ions. Therefore Al2O3 acted as network former [8, 9]."

Jan 1, 2011

By S. R. Reddy, R. G. Reddy

"The Margules equation is used for interpreting excess Gibbs energy of several ternary systems. In the present study activity coefficient of a dilute solute, 2, in a binary solvent 1-3 was derived. The derived expression is used to interpret logarithmic activity coefficient of oxygen and sulfur in several metallic systems. Self interaction parameter of the solute is derived from the partial function of solute using constant compositional path. An expression for logarithmic activity coefficient and self - interaction parameter of solute is also derived using Maclaurin infinite series. The derived equation is based on Maclaurin infinite series used successfully to deduce thermodynamics of self interaction of oxygen as a interstitial atom in two metallic systems. The predicted thermodynamic parameters values using Maclaurin infinite series and Margules equations, are in excellent agreement with the experimental data and also our predictions are far more accurate than the predictions made by other models.1 IntroductionIn most of the pyrometallurgical high temperatures processes, interactions of solutes such as oxygen, nitrogen and sulfur, with the solvent atoms are most important during refining processes. There are numerous theories are developed [1-25] to interpret the thermodynamics of solutes in multicomponent alloy systems. Which are mainly developed using statistical or Quasichemical equations.Wagner [4] developed one energy parameter ideal solvent model based on activity coefficient of solutes compositional dependency. He used one energy interaction term which is not able to account for interaction energy parameters for the same solute concentration at different solvent compositions and also it is ineffective model to predict for strong interacting systems."

Jan 1, 1996

By A. E. M. Warner

Inco Limited has long and extensive experience in converting nickel-copper primary smelting mattes over a broad range of nickel/copper weight ratios and combined nickel-copper-cobalt contents. At the Copper Cliff Smelter, the composition of the converter product matte has to meet the requirements of the matte separation process; at the Thompson Smelter, converter matte of a different composition is cast into anodes for nickel electrorefining; and in Soroako, Indonesia, a very low copper product matte is granulated for the Japanese market. Recently, Inco has conducted pilot plant testing of three possible nickel-copper matte continuous converting routes, namely flash converting, oxygen top blowing-nitrogen bottom stirring, and tuyere blowing. This test work has generated substantial new information on nickel-copper matte converting chemistry. This overview paper reviews the metallurgy of nickel-copper matte converting, in particular the behaviour of cobalt and the operating conditions required to meet the iron and sulfur specifications of the product matte. The relevant thermodynamic information is used to discuss the industrial data.

Jan 1, 2003

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 Milton Blander

A review of concepts and theories for predicting thermodynamic solution properties of multi- component high temperature liquid solutions is reviewed. During the last 50 years the ability to predict :such properties for molten salts, silicates and metals based on the generally known properties of the lower order (often binary) systems has been developed and shown to provide predictions which are quite useful in science and technology. There are many gaps in our understanding of these high temperature solutions, especially for metals, and considerably more work is needed.

Jan 1, 1996

By Agnes Y. Lee

he U.S. Bureau of Mines developed a method to treat lead-contaminated soil and ebonite battery casing wastes to produce a nonhazardous material. The cleanup procedure involves wet screening to separate a minus 18-mesh soil fraction; removal of metal1ic lead, rocks, wood, etc. ; carbonation to change lead sulfate to acid-soluble lead carbonate; size reduction; acid leaching; and rinsing. The casing wastes undergo size reduction and washing to remove the lead sulfate sludge before carbonation. Similarly, the minus 18-mesh soil is carbonated, then acid leached and rinsed. In leaching, fluosilicic acid (H SiF,) and hydrogen peroxide (H20,) are used to dissolve lead compounds. An electrowinning method is employed to strip lead from the lead-rich leachate. The acid content in the leachate is replenished with fresh H,SiF, acid prior to recycling. Treated casing wastes and soils pass the Toxicity Characteristic Leaching Procedure (TCLP) test and can be reclassified as nonhazardous materia1s. Based on this process, a conceptual pilot plant has been designed which will be demonstrated on wastes from two Superfund sites.

Jan 1, 1993

By I. Goy D. Gaballah

Decontamination of synthetic K2Cr2O 7 solutions containing 10 to 1000 ppm of hexavalent chromium using chemically treated barks have been studied at a laboratory scale. Metal removal from solutions depends on the pH, the initial concentration and the bark species. The use of a pulp density of 2 % in an agitated flask at the optimum pH for 2 hours leads to a percentage chromium removal of about 95 of the initial metallic ions content. Other trials conducted by column percolation permit the determination of the maximum retention capacity of the treated bark. Depending on the bark species, oak or pine, the rate of saturation is 110 and 215 mg of Cr per gram of bark respectively. The incineration of the metal charged barks gives recyclable, ashes containing 36 and 54 % of chromium metal for the oak and pine barks respectively. Experiments, of Cr6+ removal from industrial effluents containing up to 1800 ppm have been carried out on the semi-pilot plant scale. They have lead to the elimination of about 90 % of hexavalent chromium from this industrial waste solution. Further studies are conducted in order to define the hexavalent chromium binding mechanisms on bark constituents.

Jan 1, 1992

By Duan Xin-hui, Wang Xin, Peng Jin-hui, C. Srinivasakannan, Zhang Li-bo

The work attempts to optimize the process of preparation of modified semi-coke from semi-coke using phosphoric acid (H3P04) as the activating agent using the response surface methodology (RSM). The influences of three major dependent variables, the impregnation ratio, activation time, and activation temperature were assessed on the independent variables yield and the iodine number. The empirical relationship between the dependent and the independent variables were established using the quadratic response surface models, which were utilized to optimize the process parameters. The significance of each of the parameters and interaction among the parameters on the independent variable was assessed based on analysis of variance (ANOVA). The process variables were varied within the range of impregnation ratio (IR) from 1.5 to 4, activation time from 30 to 90 min and activation temperature from 550 'C to 650 'C. The optimized process conditions were estimated to be an IR of 2.29, activation time of 32 min, and an activation temperature of 605°C respectively using the process optimization tool. The BET surface area of modified semi-coke of the optimized sample was estimated to be 915m2/g, with the pore volume of0.71cm3/g, with an average pore diameter of 3.09 nm, with micropore volume fraction being 52.36%. The scanning electron microscope (SEM) images were utilized to visualize the surface pore structure.

Jan 1, 2013

By S. Agatzini-Leonardou

The objective of this work was to prove repeated loading capacities and investigate the selectivity of physically stabilized algal biomass from Spirulina platensis and Chlorella sp. for the removal and recovery of cobalt, nickel and chromium from laterite heap leach liquors. The testwork was carried out on a bench scale in small glass columns and proved that it was possible to immobilize the biomass on the highly porous surface of pumice stone (kissiris). Nickel and cobalt could be removed from pure aqueous solutions of each metal by the immobilized cyanobacterial biomass. Nickel and also cobalt biosorption was sensitive to the initial solution pH. Cobalt recoveries up to 80% were achieved after 5 loading cycles, from low concentration solutions, at pH 6.0. Nickel removal was complete under the same conditions, whereas chromium sorption was ineffective. Desorption of the metal loaded columns was effected by dilute sulfuric acid. The algal species giving the best adsorption capacities for the metals under consideration was selected for further experimental work with real laterite heap leach solution produced by column leaching. A statistical analysis of all obtained results was conducted using the fraction of metal removed as response. The ratio "mass of metal removed to mass of protein contained in the immobilized cells" was determined as well. The described method might be applicable for recovery of cobalt and nickel from diluted laterite heap leach solutions, such as heap wash waters, or for their removal from waste streams of a hydrometallurgical extraction process.

Jan 1, 1997

By Musa Karakus

The sedimentary iron ores of Alsace-Lorraine, France have very high phosphorous contents that average 0.7% and are as much as 2.19% P. Ores from the Tucquegnieux and Joeuf mines have been studied by cathodoluminescence microscopy, X-ray diffraction, scanning electron microscopy, and electron microprobe analysis in order to fully characterize the mineralogy, size, shape, and distribution of the deleterious phosphate grains. The phosphorous occurs as collophane, a carbonate fluorapatite, in ten morphological forms, most abundantly as microcoprolites, but also as intraclasts, concentric layers, and cortices in ooids, phosphate replaced ooids and bioclasts, phosphatiC shells, fossil infillings and internal molds, fish teeth, phosphatiC laminae, and cements between the goethite ooids. About 95% of the phosphate grains are sufficiently large that relatively fine grinding fol'lowed by reverse flotation would be expected to be effective in significantly diminishing the phosphorous content of the concentrates.

Jan 1, 1989

By J. E. Dutrizac

Fracture-exposed surfaces of sphalerite samples having five different solid solution iron contents ranging from 0.0 wt% to 14.8 wt% Fe were leached for 15 to 120 s at 100°C in 0.3 M Fe(S04)1.5 -0.3 M H2S04 media. The reacted samples were examined using X-ray photoelectron spectroscopy (XPS) which provides chemical state information on the first few nanometers of the solid surface. Surface compositions show that the leaching rate increases with increasing solid solution iron content of the sphalerite. Detailed evaluation of high resolution S2p spectra show that the leaching progresses via the formation of polysulphide species. Disulphide species were not detected in any of the experiments. Examination of the Zn2p and Fe2p spectra indicate little change in the chemical states of these elements over the duration of the experiments. Longer leaching times resulted in the generation of elemental sulphur. The ratios of elemental sulphur to dissolved ferrous ions and zinc suggest that less than 5% of the sulphide is oxidized to sulphate. Morphological studies showed that the elemental sulphur commonly formed at a few isolated sites, such as the grain boundaries. Furthermore, euhedral sulphur crystals were often identified. These observations suggest that at least part of the elemental sulphur forms via dissolved sulphide species which are oxidized in solution by ferric sulphate.

Jan 1, 2003

By William Petruk

The Kidd Creek base metal deposit near Timmins, Ontario contains around 0.15 wt% Sn, mainly as cassiterite. The cassiterite occurs largely as inclusions in sphalerite, with 85% being in grains smaller than 18.5 micrometres in diameter. Concentrates and tails from the company's Cu, Pb and Zn circuits were studied to determine the liberations and recoveries of cassiterite in the products. The ore had been ground to about 65.% minus 44 micranetres in diameter (-325 mesh); 55% of the cassiterite was liberated. About 92% of the liberated cassiterite and 70% of the unliberated cassiterite were in the concentrator tails, and 20% of the unliberated cassiterite in the zinc concentrate. The company had attempted to recover the cassiterite from the concentrator tails by gravitational methods but recoveries were low. The grain size of the cassiterite in the gravity Sn concentrate was similar to the grain size of the liberated cassiterite in the concentrator tails. Research on flotation of the fine grained cassiterite from Kidd Creek ore has been conducted,

Jan 1, 1990