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By Patrick R. Taylor

This investigation studied the inflight calcination kinetics of nuclear waste simulant using a thermal plasma reactor. A series of experiments were performed to determine the conversion of insoluble aluminum compounds to the soluble compounds and the decomposition of complex organic and nitrite compounds present in the simulant waste. Thermodynamic calculations based on free energy minimization were performed to establish a theoretical basis for this investigation. A kinetic model to describe the conversion of gibsite to sodium aluminate has been proposed. The products of the calcination were characterized using XRD, Gas Chromatography, and chemical analysis by ICP. The results of this investigation indicated 85% gibsite conversion to sodium aluminate, 90% of nitrate decomposition, 52% TOC decomposition and 90% conversion of chromium to soluble compounds. A process is identified for inflight calcination of wastes. Key words: Plasma, waste, simulant, calcination

Jan 1, 1996

By P. Klut, D. Groult, R. Marechalle, B. T. H. Bonnema

In the past 5 years, Compagnie Europeenne de Dezingage (CED) has developed a successful dezincing process and the St. Saulve pilot plant has evolved into a commercially successful production plant. Currently the plant meets all the required standards for scrap and zinc quality, output capacity, availability, and meets the prescribed environmental emissions standards. The initial process problems relating to zinc recovery, uncontrollable explosions and sodium hydroxide aerosol emissions have all been solved. Presntly, the yearly production of dezinced scrap is around 50.000 tonnes/year; this capacity is enough to supply the local market. This capacity can be increased easily to 65.000 tonnes/year or more. The market for dezinced material is growing due to the increased consumption of galvanized material on one hand and on the other hand the higher demand for high quality scrap. The proven technology of CED is currently patented worldwide, but CED is inviting licensees to implement the dezincing technology in other parts of the world.

Jan 1, 2000

By Lawrence L. Brown

As part of the Federal effort to help maintain an adequate supply of fertilizer materials, the Bureau of Mines conducted research to characterize complex low-grade Michigan phosphate materials and to devise methods for recovering fertilizer-grade phosphate concentrates. The rock is from middle Precambrian sedimentary formations in the Marquette Range located in the central part of the Upper Peninsula of Michigan. Occurrence of phosphate-bearing sediments in Precambrian rocks is rare. This deposit, containing 12 to 15 pct P2O5 is believed to be the richest Precambrian phosphate deposit in the United States. Petrographic examination showed that the conglomeritic rock contains crystalline apatite both in "black pebbles" and in quartz matrix. Attrition scrubbing and sizing tests showed that there is no tendency for phosphate to concentrate in any of the sized fractions. In beneficiation tests, which included grinding to minus 325 mesh followed by phosphate mineral flotation using a fatty acid-fuel oil collector, a phosphate concentrate was obtained that had a grade of 30 pet P2O5 and a P2O5 recovery of 72 pct. This concentrate should be suitable for fertilizer manufacture.

Jan 1, 1982

By B. Manana

In heap leaching, the oxidative dissolution of value minerals encapsulated deep within large particles cannot be fully understood on the basis of the bulk solution conditions relative to variable solution conditions near the mineral surface. In the present study, the diffusion of the oxidising species through inner particle pores is simulated in a model apparatus that separates an inert platinum electrode under controlled reduction potential from the bulk solution through narrow pores of varying length. The Cu-NH3 system was selected as a model system and Cu(II)/Cu (I) as the redox couple of interest. Platinum probes inserted in the pores allowed the measurement of varying redox potentials along the pore length. Results showed that in a 10 mm pore, there exists a narrow (0.5 mm) zone near the reduction surface that is depleted of the oxidant and in which its supply is strongly diffusion limited, even if it is in abundance in the bulk solution. The consistent presence of this narrow diffusion region across all experimental results indicated that the transportation of the reduced species away from the reaction surface had the most significant influence on the potential variations within the pore. This was further supported by the minimal effect of varying concentrations of both Cu(II) and dissolved oxygen on the solution potential within this region.

By C. J. Parradies

During injection into a die, semi-solid metal alloys exhibit a shear-rate, history-dependent flow response. Simulating the injection of a thixotropic material requires that empirically determined boundary conditions and viscosity are specified as a function of both temperature and shear rate history. Experiments were performed using an industrial die casting machine that was instrumented with sensors to measure the pressure and temperature during the injection of a semi-solid aluminum alloy through a tube. This benchmark experiment was used to develop a simulation of the die casting process that could then be applied to more complex die geometries. The results of the experiments were analyzed using the exact, steady state solution for a power law fluid and simulations accounting for slipping at the boundary between the semi-solid metal and the die. Results indicated that the no-slip condition cannot be used to simulate the velocity boundary condition, because the measured pressure is much lower than that predicted by the models. An estimated apparent slip coefficient was introduced to account for the reduced pressure. During some of the experiments, a sudden drop in the measured pressured, prior to decreasing the ram velocity, coincided with observations of segregation in the form of concentric rings visible on the polished surface of cross-sections cut from material remaining in the tube.

Jan 1, 1997

By David R. Jessey

An ore microscopic and geochemical study of the nickel-cobalt occurrence in the Southeast Missouri Mining District has revealed several significant relationships. Siegenite [(Ni,Co)3S4] is the dominant nickel-cobalt sulfide in the ores, however, several other members of the thiospi¬nel group (AB2S4) occur: carrollite (CuCo2S4), nickelean carrollite [(Co,Ni,Cu)3S4], fletcherite [Cu(Ni,Co)2S4] and polydymite (Ni 3S4). In addition, bravoite [(Ni,Fe)S2], vaesite (NiS2), millerite (NiS) and gersdorffite (NiAsS) are present. Thiospinel composition varies dramatically within the district. Paragenetic studies have shown that the stratigraphically lowest thiospinels are the most cobalt-copper-rich. A detailed ore microscopic study of the AMAX Lead Company Buick mine has also shown significant changes in mineralogical association, texture and grain size of the siegenite along the north-south strike of the major ore bodies. Siegenite commonly replaces and veins chalcopyrite and is subsequently replaced by sphalerite. Less commonly, siegenite and chalcopyrite are observed to form linear replacements along sphalerite grain boundaries. The grain size of the siegenite varies markedly, but in a predictable north-south pattern that is consistent with a genetic model formulated from geo-chemical data. The compositional as well as textural trends displayed by the thiospinel mineralization could be exploited to optimize recovery of any or all thiospinels of economic interest.

Jan 1, 1981

By J. E. Dutrizac

The mineral forms of silver, lead and cadmium in the zinc concentrates and the various roaster products made by the Kidd Creek Division of Falconbridge Inc. have been elucidated. In the concentrates, all three elements occur mainly in sulphide form, either in solid solution in the principal ore minerals or as discrete mineral grains. During roasting, Ag, Pb and Cd are preferentially concentrated in the hot cyclone and ESP dusts of the roaster train. Silver is converted to <0.5 µm grains of silver metal and to Ag2S04 which dissolves in or impregnates silicates. Lead is converted to Pb-bearing silicates or to PbS04 and PbO which are present either as tiny free grains in ZnO or as an intergrowth with lead silicate. Lead is also a minor constituent of the ferrite phase. Cadmium occurs mostly as cadmium-bearing zno and ZnFe2o4 , but a significant amount also reports as Cd-bearing silicates or zinc sulphate.

Jan 1, 1990

By D. J. Senor

Closed chamber incineration (CCI) is a novel technique by which irradiated nuclear graphite may be destroyed without the risk of radioactive cation release into the environment. The process utilizes an enclosed combustion chamber coupled with molten carbonate fuel cells (MCFCs). The transport of cations is intrinsically suppressed by the MCFCs, such that only the combustion gases are conducted through for release to the environment. An example CCI design was developed which had as its goal the destruction of graphite fuel elements from the Fort St. Vrain reactor (FSVR). By employing CCI, the volume of high level waste from the FSVR will be reduced by approximately 87 percent. Additionally, the incineration process will convert the Sic coating on the FSVR fuel particles to SiO2, thus creating a form potentially suitable for direct incorporation in a vitrification process stream. The design is compact, efficient, and makes use of currently available technology.

Jan 1, 1994

By Serdar Aksu, Fiona M. Doyle

"CMP will be an essential process in the production of integrated circuits containing copper interconnects. This study aims to improve our mechanistic understanding of the role that organic chelating agents might play in the reactive slurries used in copper CMP. Copper dissolution behavior in EDTA arid glycine was first examined by producing potential-pH diagrams for the copper-water-EDTA and copper-water-glycine 'systems. The results of potentiodynamic polarization experiments were then considered in light of these diagrams. . In-situ polarization experiments were conducted to gain insight into the electrochemistry of copper during dynamic polishing in slurries prepared from EDT A and glycine.IntroductionCopper has recently started to replace aluminum as the interconnect metal in integrated circuits. Copper interconnection offers faster and more reliable integrated circuits due to its higher electrical conductivity and superior electromigration resistance (1). The damascene method is used to form multilevel interconnects in the manufacture of integrated circuit devices with copper metallization (2, 3). Copper is deposited by CVD or electroplating into vias and trenches etched in the interlayer dielectric (IDL), over a diffusion barrier usually made from titanium, tantalum or their nitrides. Chemical mechanical planarization (CMP) then prepares the wafer for the next deposition step, by removing excess copper and planarizing the surface. During CMP, the wafer is rotated and pressed against a rotating platen covered with a polishing pad. Chemically active slurries containing submicron size abrasive particles (Si02, Al20 3, ceria, diamond, etc.) are applied. Both the mechanical action of the abrasive particles and the chemical action of slurry constituents remove material from the wafer surface. Planarization results because material is removed faster from protruding regions on the surface than from recessed regions. Since CMP can globally planarize .the entire wafer, it has become one of the key technologies for producing integrated circuits with copper metallization."

Jan 1, 2000

By Beate Ina Jenssen

Ferric iron removal from the nickel electrolyte at Glencore Nikkelverk AS in Kristiansand, Norway, is achieved by precipitation of iron hydroxide followed by filtration, and it is desirable to improve filtration properties of the precipitated iron hydroxide in order to decrease the filtration time. The effect of increasing the residence time from the current 45 min to 75 min and temperature from 65 °C to 90 °C on the filtration properties of the precipitated iron hydroxide (akaganéite) was studied by simulating the industrial process conditions in a continuous reactor setup operating at steady state, using ferrous-containing process solution as feed material. It was possible to decrease the filter cake resistance by both increasing residence time and temperature, but temperature gave the most pronounced effect and reduced the filter cake resistance by one order of magnitude.

By Michael J. McGuire

Rostoker, Inc. has developed a process to smelt solid hazardous/non-hazardous inorganic wastes. Near seven hundred experiments were performed. Actual industrial wastes as well as reagent grade chemicals were used. By mixing a multiplicity of these wastes to proper formulations, then furnacing them, it was determined that saleable end products could be reclaimed; metal, fume and slag. The slag, due to its siliceous structure was tested to be leach resistant (40 CFR). This formed the essence of our patent, #5,180,421 "Method and Apparatus for Recovering Useful Products from Waste Streams". What is unique is that a HTMR (High Temperature Metal Recovery) process has been developed that can treat a multiplicity of wastes within the same furnace. The discussion will include a list of waste streams we have treated, details of proper waste formulation and experimental results.

Jan 1, 1994

By David N. Hanlon

The effect of high-temperature plastic deformation of the austenitic phase (y) on the subsequent phase transformation to ferrite (a) has been experimentally investigated, and modelled using a physically-based model. The effect is of importance for steel sheet, in view of me significance of the phase transformation with respect to the eventual properties of the material. In this paper the kinetics of the y ? a phase transformation has been studied after different degrees of prior deformation. The degree of deformation is varied by applying different deformation temperatures and strain rates, and by allowing a varying extent of recovery and recrystallisation. Consequently, both dynamic and static recovery and recrystallisation have been involved. The dilatometric observations on the phase transformation have been modelled using an interface-mobility model, in which the effect of the dislocation structure is introduced as an additional driving-force term. The effect of the stored energy on the nucleation process, which appears to be affected more strongly than the growth of ferrite, is examined in terms of the classical nucleation theory.

Jan 1, 2001

By Gil Bourcier

A process has been developed for detoxifying spent potliner (SPL) in which the SPL is blended with limestone and an anti-agglomeration agent and thermally treated in a rotary kiln. The process has been proven and a commercial plant is in operation at Gum Springs, Arkansas. The treated by-product material has been delisted by the U.S. EPA and is now a potential raw material for many commercial applications. Finding uses for a non-hazardous material has many advantages over finding uses for a hazardous material like SPL. Complete usage of the by-product will complete the life cycle and eliminate any landfilling of non-hazardous SPL by-products or residues. Being non-hazardous and containing compounds used in the ceramic and numerous other industries assures many potential uses for the spent potliner by-product.

Jan 1, 1994

By T. C. Goel, A. Venna, R. G. Mendiratta

"Processing of ferrites has gained tremendous importance in recent times to meet the high performance demands on ferrites in keeping with the fast emerging· technologies. The quality of ferrite powders has strong influence on ·the performance of final device. Fabrication· of high performing ferrite components requires starting ferrite powders of precise stoichiometry, purity and microstructure. It is difficult to obtain these attributes by the conventional ceramic method. The key to obtaining quality powders lies in the· solution techniques. With this in view soft ferrites have been prepared by a wet chemical process, known as the citrate precursor method, which involves the formation of citrate complexes of the constituent cations. The advantages of this process are the ease of preparation and close control of composition, homogeneity, purity and particle size. Electrical and magnetic measurements on lithium ferrites have shown resistivity higher by more than two orders of magnitude compared to that observed for samples prepared by the conventional ceramic method, and low magnetic losses, making the ferrites specially suitable for high frequency applications.IntroductionProperties of ferrites are known to be sensitive to .their processing technique. A small deviation in the compositional stoichiometry of the ferrite affects its properties greatly. Soft ferrites such as Ni-Zn, Mn-Zn and Mg-Mn. are well known ferrites covering wide-ranging applications [1,2]. Lithiiim ferrites have also assumed technological importance for microwave applications and are potential substitutes for the expensive garnets [3]. Lithium ferrites are often doped with zinc to tailor the saturation magnetization required at high frequencies. Lithium and lithium-zinc ferrites, however, present difficulty to processing due to the volatile nature of both the cation components, namely Li and Zn. These ions are volatile at temperatures > 1000°C which makes their processing difficult. One of the main considerations of high frequency performance of ferrites is the high eddy current losses which prevent the interaction of the magnetic field with the ferrite component and hence impair device performance. These losses can be reduced by having a material of high resistivity. Electrical conductivity in lithium ferrite has been attributed to electron hopping [4] between the two vaience states of iron, Fe2+ <=> Fe3+, on octahedral sites. Maintaining the + 3 valence state of otahedral- Fe ions is thus a prerequisite for achieving high resistivity. The resistivity of ferrites is normally found to be low when processed by the conventional solid-state or the ceramic method [5]. This is attributed to (a) extensive ball-milling employed in the method to mix the component oxides results in non-stoichiometric compositions due to introduction of additional Fe ions on abrasion of steel balls during milling, (b) high processing temperatures involved which result in significant volatilization of Li and Zn ions creating thereby oxygen non-stoichiometry which results in reduction of Fe3 + to Fe2 +, (c) large and non-uniform grain sizes. In the present work, preparation of Li and Li-Zn ferrites by a non-conventional method known as a citrate precursor method [6, 7] which requires lower processing temperatures and duration is reported. The method gives stoichiometric compositions on account of homogeneous atomic-scale mixing of the constituent cations via the formation of metal-citrate complexes mixed in solution state. The method is also capable of giving small grain size which aids the oxidation ofFe2+ ions."

Jan 1, 2000

By Gabriel Riveros, Ariel Balocchi, Andrzej Warczok, Daniel Smith

Blister copper from converting of copper matte is processed by fire refining prior to electrorefining. The fire refining consists of two steps: copper oxidation with impurities slagging and copper reduction. The classical batch process is carried out in vascular or reverberatory furnaces called anode furnaces. A new process for continuous copper fire refining has been proposed. The copper flows through two reactors in cascade, where is oxidized and reduced. The flow of a liquid copper through a ceramic packed bed increases the surface area and the rate of oxidation as well as the rate of reduction in the packed bed of charcoal. Mathematical modelling allowed for the design of a laboratory scale demonstration installation and industrial-pilot installation in Hernan Videla Lira Smelter (Paipote). The results have demonstrated the process feasibility and flexibility in operation.

Jan 1, 2009

By Mark H. Hashiguchi

Examination of tensile bar surfaces shortly after destructive testing was conducted to search for clues that would aid in optimization of mechanical properties, especially tensile strength, yield strength and elongation to fracture. Cu-Ni-Si-Cr alloy bars in the as-cast, forged, rolled and extruded conditions were examined. Low ductility bars (<4% Elongation) showed dramatically different features than the fracture surfaces of high strength - high ductility bars (7 to 10% Elongation). Analysis of the fracture surfaces at 15X to 2000X and use of Energy-Dispersive X-Ray Spectroscopy (EDS) identified Ni-Si and Ni-Si-Cr precipitates of varying sizes and morphologies. Thermo-mechanical processing techniques to control the size and distribution of these precipitates show promise in improving the properties and performance of this alloy system and appear to correlate with improvements in the fracture surface morphology.

Jan 1, 2008

By Hui Wang

With the great increasing use of nickel metal hydride batteries recently, the waste of this kind batteries have been paid for close consideration. For the main reason that the waste of the batteries contained precious metals and lanthanide which cost great lose. This paper introduces the pyrometallurgical process of recovering nickel and cobalt from the waste of the nickel metal hydride batteries. Particularly, the waste for the process was from factory during the producing program. The use of designed solvent to divide nickel and cobalt in melted state from the waste is described. Also, the result of the nickel and cobalt and melted gangue that mainly consist of lanthanide oxide are included in details. The aim of the paper is to find out a simple and feasible way to reuse waste from nickel metal hydride batteries.

Jan 1, 2009

By Zhao-cheng Liu

Iron oxide red pigment powders of high quality were synthesized from pyrite cinders. Iron ox-ide red pigment powders were synthesized by hydrothermal method from the precursor of Fe(OH)3 and Fe(OH)2 colloid, which were obtained after ammonia solution reacted with acidic leaching solution produced by the reaction of pyrite cinders with sulfuric acid. Effects of reaction concentration, reaction temperature, reaction time, pH value and n(Fe2+)/n(Fe3+) on main properties of oxide iron red were studied by experiments. The prepared particles were characterized by means of X-ray diffraction (XRD) and scanning electron microscope(SEM). The results revealed that the synthesized iron oxide red particles were _-Fe2O3 and pseudocubic with particle size of 0.50~0.75µm. Furthermore, the quality of iron oxide red pigment powders reached the first grade of national standard (GB1863-89 ).

Jan 1, 2009

By S. Neven

The smelting of copper anode slimes, a material which contains mostly lead, silver, copper and selenium, has been practiced for many years with a view to recovering the silver and associated small amounts of gold. However, a theoretical understanding of the process has been lacking and this handicaps efforts to improve and intensify smelting operations. In the past few years work has been done in this area and this work will be reviewed in the paper. The underlying thermodynamics of the oxidation of silver-copper selenide mattes has been developed and used as a basis for the construction of a computational thermodynamics model which attempts to predict the composition of all condensed phases during the course of smelting. The model will be outlined and its successes in matching experimental data, as well as its current deficiencies, will be considered. Supporting work on the thermodynamics of silver solubility in slags, on activity-composition relationships in the Ag-Se system and work in progress on the oxidation state of copper in the slags will be reviewed. These projects are designed to provide further detailed data which will improve the robustness of the thermodynamic model.

Jan 1, 1999

By A. Jakobsson

Studies of the rate of interdissolution in oxide systems in the solid state are of importance in materials processing through the powder-metallurgical route. As there is a need for following the rate of the such reactions continuously, a new method based on high temperature X-ray diffraction was developed. Mechanical mixtures of the oxides were placed in a high-temperature X-ray diffraction unit and the changes in the intensity and position of the peaks with highest intensity for both the components were followed as functions of time. A suitable theoretical model has been developed in order to interpret the experimental data and evaluate the diffusion coefficients. The method was applied in the case of the system MgO-NiO. The results obtained are compared with those obtained by another new method, based on solid-state galvanic cell technique with calcia stabilized zirconia electrolyte, developed in the Department of Theoretical Metallurgy. The advantage of the present techniques to monitor the progress of the reaction continuously make them suitable for computer control of such processes.

Jan 1, 1995