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By H. L. Fraser

A review of the possibilities of performing microchemical analysis in thin sections using a combination of scanning transmission electron microscopy and energy dispersive spectroscopy of x-rays is given. Particular attention is paid to the factors that limit accurate analysis at the highest spatial resolution. As an example of the use of these techniques applied to a potential problem in minerals processing, the identification of iron pyrite and pyrrhotite particles in Illinois, Herrin #6 coal is presented.

Jan 1, 1981

Pyrometallurgical reactors constitute a key processing component in the total primary and secondary resource cycle, being involved both in primary smelting, converting and extraction, as well as the reprocessing of scrap, from aluminum cans to end-of-life automobiles. To effectively control the overall resource cycle, one needs to take a systems modeling approach of the whole cycle, seeking to also understand the dynamic process behavior of the individual components of the cycle, and then especially the part that contributes most to the chemical conversion, namely the pyrometallurgical reactor. This paper highlights the role of pyrometallurgical thermodynamics, in the whole resource cycle and specifically places equilibrium thermochemistry in the context of process dynamics where large variable inventories are recycled or maintained within the system. This paper will therefore review the semi-empirical dynamic modeling tools, which are used to model complex systems with the specific goal of developing dynamic predictive models, which also include slag-alloy chemistry, towards controlling the recycling in a feed forward manner. To illustrate the primary processing side, high carbon ferrochrome will be presented as a brief case study. It also will show how the distributed nature of the chemistry of melts in the case of primary extraction, and secondary materials such as recycled end-of-Iife vehicles, have a significant impact on the process outcomes and model predictions. It is therefore argued that the fundamental thermodynamics and kinetics in metallurgical reactors playa final crucial role in modeling the closed material cycle, but only when it is used in conjunction with process systems theory based on reconciled data for parameter estimation and model calibration.

Jan 1, 2003

By L. Yin, R. B. Haber, N. Sobh, D. A. Tortorelli, R. W. Hyland Jr.

"We optimize continuous quench process parameters to produce a desired precipitate distribution in aluminum alloy extrudates. To perform this task, an optimization problem is defined and solved using a standard nonlinear programming algorithm. Ingredients of this algorithm include a cost function, constraint functions and their sensitivities with respect to the process parameters. These functions are dependent on the temperature and precipitate size which are obtained by balancing energy to determine the temperature distribution and by using a reaction-rate theory to determine a discrete precipitate particle size distribution. Both the temperature and the precipitate models are solved via the finite element method. Since we use a discrete particle size model, there are as many as 105 degrees-of-freedom per finite element node. After we compute the temperature and precipitate size distributions, we must also compute their sensitivities. This seemingly intractable computational task is resolved by using an element-by-element discontinuous Galerkin finite element formulation and a direct differentiation sensitivity analysis which allows us to perform all of the computations on a PC.1 IntroductionThis work addresses the need for an integrated design capability that links microstructure evolution to the process parameters. It is motivated by the manufacture of lightweight aluminum-alloy extrusions for use in automotive structures. Aluminum alloys offer obvious benefits, however, care must be taken to manufacture favorable microstructures that ensure acceptable structural performance. For example, the manufacturing process for 6000-series components involves hot extrusion of cast aluminum billets followed by either an air or water quench process. The bill~t's initial grain structure is dramatically altered during extrusion by massive mechanical deformations and recrystallization processes. The microstructure continues to evolve during the quench, as complex chemical processes determine the formation of precipitates. The control of the precipit'ate size distribution is vital. Indeed, large precipitates located on grain boundaries serve as crack initiation sites which adversely effect structural crash· worthiness."

Jan 1, 2000

By Joon H. Jang

At a selected pH, hydrothermal oxidation of chalcopyrite was carried out under controlled F+,, at elevated pressures and temperatures (172-200°C) by balancing the rate of oxygen injection against the rate of consumption. Chalcopyrite was converted to covellite (CuS) and digenite (CU1.8S) with rejection of iron and sulfur to the solution. Covellite forms in the first stage, followed by nucleation and growth of digenite in the second stage. The effects of rapid and slow injection of stoichiometric quantities of oxygen are compared. Both the covellite and digenite form a porous layer occupying the same volume as the original chalcopyrite grain. An electrochemical kinetic model is presented to correlate the observed results.

Jan 1, 1993

By Raymond E. Healy

Mercurian e1ectrum (Au-Ag-Hg alloy) is the principal Au-bearing phase in the massive sulphide ores at Trout Lake, Manitoba. The average composition of this phase (in wt %) is 49.2 % Ag. 38.7 % Au and 11.0 % Hg, with ranges of 17.34 to 76.47 % Ag, 1.62 to 79.86 % Au and 1.29 to 30.87 % Hg. Compositional variation reflects solid solution in the a-phase of the Ag-Au-Hg system. Backscatter electron imagery reveals systematic zoning and suggests a general crystallization sequence from metamorphic pore fluids of progressively Ag-rich compositions. Investigation of the occurrence of gold in mill products demonstrates that mercurian electrum accounts for over 90 % of the Au in Trout Lake ore. I Invisible" gold in pyrite (x = 0.72 ppm Au) and arsenopyrite (x 30.2 ppm Au) is confirmed by SIMS analyses, and accounts for 7-10 % of the Au in the ore, and 35 % of the Au lost to the tailings. The remaining 65 % of the Au lost to the tailings consists principally of mercurian electrum locked with pyrite. No significant losses of mercurian electrum in the size range amenable to flotation and/or regrinding is indicated.

Jan 1, 1989

By Paula Ana Paiva

The high economic value and unique technological properties of the platinum-group metals (PGMs), plus their growing scarcity in the Earth’s crust, justify the crucial importance of developing recycling practices for PGMs end-of-life materials. Examples of top devices relying on the use of PGMs are automotive and industrial catalysts, and electrical and electronics equipment. This article critically describes the most recent research on the use of solvent extraction to recover one PGM, palladium, from spent catalysts. Some groups focus on the development of schemes involving commercial extractants, while others prefer to design specific molecules to efficiently and selectively recover palladium from these particular complex leaching solutions. Examples of commercial extractants proposed for the former schemes are Alamine® 308, TBP and LIX® 84I; while on the other hand, sulfur-containing diamides, thioamides, thiocarbamates, and dithioethers have recently been developed. Ionic liquids have to be mentioned too.

By H. Shang

The materials science and metallurgical engineering communities have expended enonnous resources in developing high fidelity process models. Exploiting these Models for Predictive Optimization (MPO) and Control (MPC) is a new frontier in Materials Process Engineering that will lead to exceptional process perfonnance. This paper will begin with a short survey of the development of high quality process models available in the literature and a discussion of how these could be used to improve process operation. A summary of the current "state-of-the-art" in process automation technologies and the traditional framework in which these technologies are deployed will be presented. An illustration of the use of MPO in process design and operations will be presented for the continuous casting of steel. In addition, a simple run-out table simulation will be used to demonstrate the power of the MPC technique.

Jan 1, 2003

By J. B. W. Bailey

The Noranda Horne smelter in Quebec, Canada has change considerably during the last two decades to accommodate varying custom concentrate receipts, closure of the Horne mine, better working conditions, environmental programmes, new technology and increased energy and labour costs. This paper highlights the reasons for changing the smelter from two calcine charged and one wet charge reverberatory furnaces fired by coal to a smelter using. tonnage oxygen oil, natural gas and coal in a single wet charged reverberatory furnace and a Noranda Process continuous Reactor. The current operation 1 described, including three major topics; the use of oxygen/fuel burners on the charge banks of the reverberatory furnace which has increase the smelting rate from 680 to 1100 tonnes of concentrate per day; the oxygen enrichment of the Noranda Process converting air to achieve smelting rates of over 1800 tonnes of concentrate per day; the converting of the mixture of 73 percent copper matte produced from the Noranda Process and the 33 percent copper matte produced from the reverberatory furnace.

Jan 1, 1983

By C. Gasparrini

Mineralogy may be applied to the selection of appropriate separation techniques, as well as to assist in the evaluation of problems causing loss of metals and other economically important elements during plant processing. Mineralogic studies may thus help develop techniques to optimize metal recoveries. The present paper describes how such factors as the minerals in which the elements of interest are concentrated, their chemistry, the chemistry of the associated minerals, grain size and textural associations with other minerals in the ore, may affect decisions on separation techniques for the recovery of economic elements. A number of case studies are described in which the mineralogical observation of ore samples has revealed the cause of problems experienced in the extraction of select precious and base metals, or has been decisive in the choice of appropriate techniques for recovery.

Jan 1, 1981

By Akio Ohta

The Hyuga smelter has been producing ferronickel by a rotary kiln-electric furnace process in Miyazaki, Japan. Several approaches to improve our operation have decreased the electrical energy consumption. A new process was developed to decrease the cost of energy even further. Oil and technical oxygen are injected through lances to heat up the calcined ores (calcine) instead of the electric power. Main problems during the development of the process were the short life of the water-cooled lances, the check on security of the safety system and the eruption of combustion gases through the calcine bed. These problems have now been overcome successfully, and stable operation can be maintained. The addition of 1 Litre of heavy oil per tonne of ore can save the electrical energy requirement by 8.6 kwh per tonne of ore. The new process has resulted in a reduction of the electrical energy consumption by more than 10 percent

Jan 1, 1992

By Jr. Napolitano, Jr. Sanders

"Morphological evolution of a dendritic growth front in a binary alloy is simulated using a cellular automaton approach to establish the feasibility of modeling such growth with a local rule-based scheme. The motivation for this work is derived from the need to predict the development of solidification structures within real components of complex geometry, where significant constraint of the thermal and solutal fields may exist. Such cases present complex boundaries and large domain sizes, which may preclude the effective use of more conventional methods. In this work, a model is presented which couples a two-dimensional alternate-direction-implicit finite-difference diffusion solution with a cellular automaton growth algorithm to simulate morphological evolution in alloys solidifying under directional growth conditions. Temperature, composition, and interface curvature are incorporated into a local growth potential which is used by the automaton, allowing the interface to evolve. Alloy solidification is simulated over a range of experimental conditions, producing various structures. Issues addressed include morphological instability, primary spacing selection, interface curvature, microsegregation, and tip conditions.IntroductionThe development of dendritic structure plays an essential role in alloy solidification. Virtually every microstructural feature, within a cast alloy component, is related to the interface morphology present during solidification. Conventional solidification theory, describing dendrite tip kinetics and mushy zone phenomena, provides a means for estimating overall microstructural parameters for an alloy solidified under steady-state conditions. Microstructural prediction for actual components, which are finite in size and complex in geometry, requires a description of the evolution of the interface morphology under transient conditions and geometrical constraint and an understanding of how the structure propagates through the mold. Any useful simulation tool must be equipped to handle these circumstances within the limits of computational feasibility."

Jan 1, 1998

By Jari Aromaa, Olof Forsen

"Oxygen evolution by decomposition of water is the main anodic· reaction in sulphuric acid solution. Traditional anode materials have been relatively low-cost lead alloys, though the active lead dioxide layer has a high oxygen evolution overpotential. This causes a significant increase of cell voltage. To lower total energy use in metal production, electrocatalytical properties or corrosion resistance to decrease replacement costs must be improved. Addition of an catalyzing ion will decrease oxygen evolution potential. The effective area of an anode increases by calcium additions and by producing anodes with fine microstructure. Remelting and rapid quenching is possibly a method that is economically feasible and technically simple enough to be adopted.IntroductionPermanent anodes are widely used in several electrochemical processes and cathodic protection applications. The permanent or ""inert"" anodes can be either massive or coated anodes. The massive anodes are metals, like lead alloys, or non-metals, like magnetite, graphite or ferrite. The coated anodes are made of a valve metal base (titanium, niobium or tantalum) coated with an electrochemically active coating. The purpose of anodes is to supply current to the electrochemical cell. A vast number of materials and their combinations are electrical conductors and may hence be used as anode materials. However, good anode materials must survive in aggressive environments and also be able to pass high current densities. These opposite requirements restrict the amount of possible materials. Generally, an useful anode material must meet three requirements, electrical conductivity, electro catalysis and stability. Good electrical conductivity is essential for energy efficiency. Good electrocatalytical properties are essential to improve product yield. Long term stability is also an important property, because electrode wear and corrosion may cause product contamination, increasing energy consumption and material and labor costs due to need of periodical maintenance. Electrical conductivity and electrocatalytical properties are more widely studied subjects than long term stability of anodes, and a good amount of information about these two subjects can be found in the open literature. Wear and corrosion mechanisms of the anodes vary depending on the operational conditions, i.e. concentration of different species, temperature and operating current density."

Jan 1, 1997

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 J. J. Talja

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

Jan 1, 1994

By A. Andreas Hejja

Flow of slag and settling of matte in slag resistance electric furnaces are discussed in conjunction with furnace geometries, stirring action of the electrodes, buoyancy and electromagnetic effects. The rectangular electric furnace was regarded as a channel reactor and the mode of slag flow as a channel flow. The flow is affected both by buoyancy and electromagnetic forces, however the effect of electromagnetic forces is minimal. The flow velocity is made up of two components; (i) that developed by the action of the electrodes, and (ii) the bulk flow velocity determined by the smelting rate and the volume of the reactor. Slag samples were taken from various depths of the molten bath and were analyzed microscopically to determine the size and distribution of matte particles, The action of the electrodes was described by a simple mathematical formula indicating a balanced settling rate in the area of electrode action.

Jan 1, 1996

By Sebastiaan Peelman

NdFeB permanent magnets are the best available magnets used in many technology applications. However, at their end-of-life (EoL) most of magnets and the contained REEs are lost during the recycling of the bulk metals. The REEs are classified as the most critical raw materials in the European Union, and recycling of REEs from EoL products will reduce their criticality and contribute to the sustainability of REE. Various technological routes have been reported, but most of the methods are effective for highly concentrated magnets or magnet scrap, which is greatly dependent on expensive pre-dismantling processes. This paper presents various innovative metallurgical solutions to the effective REE recovery from current industrial practice for WEEE recycling, including the ferrous scrap from WEEE shredder products and shredder residues from computer hard disk drives. Both hydrometallurgical and combined hydro- and pyrometallurgical REE recovery routes are developed after demagnetization and physical upgrading.

By Richard D. Hagni

Polished sections of pyrometallurgical intermediate products from a simulated commercial flash furnace were examined by reflected light microscopy, scanning electron microscopy-energy dispersive spectrometry and electron backscatter analysis, and microprobe analysis for phase and textural relationships. The smelter feed is a copper concentrate from a porphyry copper deposit. The concentrate consists primarily of chalcopyrite, bornite and pyrite with smaller amounts of covellite, chalcocite, molybdenite, magnetite, galena, and sphalerite. The flash furnace reactions for pyrite and chalcopyrite can be observed by reflected light microscopy. Reacted angular particles of pyrite exhibit successive rims of fibrous pyrrhotite and hematite or magnetite. Reacted angular chalcopyrite particles show successive rims of bornite, digenite, and chalcocite. Spherical particles, formed by the complete melting of former pyrite particles, consist of variable amounts of granular pyrrhotite with magnetite rims and minor hematite. Spherical particles, formed by the complete melting of former chalcopyrite particles, exhibit exsolution intergrowths with varying proportions of intermediate solid solution, bornite, digenite, and chalcocite and have rims of hematite, magnetite, and copper-iron spinel. Sphalerite and molybdenite do not show evident mineralogical reactions.

Jan 1, 1987

By N. A. Warner

Fundamental studies on the reaction of limestone or dolomite at high temperature with S02 are extended to the realm of large scale primary copper smelting. Whereas flue gas desulfurisation in the electric power utility industry is concerned with S02 concentrations normally less than 0.5 percent, high temperature smelting gases can have S02 levels approaching 100 percent. The reaction involved is very exothermic so proposals are made in this paper for returning the heat generated in sulfur fixation directly back to the copper smelting process. This integration leads to metal production with lower energy requirements than current technology. The anhydrite reaction product can either be disposed of locally with minimum adverse environmental impact or upgraded to a value-added product. It is assumed, of course, that no viable market exists to support sulfuric acid production.

Jan 1, 1996

By Gaballah Djona M.

Spent hydrorefining catalysts contain about 5 % of CoO and/or NiO, 12 % of MoO3 and up to 10 % of V205. They are generally supported by alumina and contain up to 25 percent of C, S and hydrocarbons. Such materials are potentially hazardous to the soil and to water resources. Selective chlorination of raw unroasted samples with Cl2 + air gas mixture had been investigated. At temperatures lower than 600 °C, it was possible to recover more than 90 % of nickel and cobalt chlorides, about 99 % of the molybdenum and up to 75 % of vanadium chlorinated compounds. CoCl2 and Ni/Cl2 were extracted from the chlorination residues by their dissolution with acidified water. Molybdenum and vanadium chlorinated compounds were recovered by selective condensation from the vapor phase. The chlorination of Al2O3 could be limited to less than 6 %. The scale up of this treatment was successful and a flow-sheet is proposed.

Jan 1, 1995

By Paul Van Negan

During the last decade, MHO has continued to diversify the feed. of its Hoboken smelter. The range of feed materials including larger proportions of precious metals has been extended and the production of minor metals has been developed. These diversifications have required further improvements at the smelter. Attention has been particularly focussed on an increase of productivity, compliance with emission standards and achievement of the highest recoveries of valuable elements. The assaying and sampling facilities have been considerably expanded and the different processing steps of the smelter are now also systematically controlled and managed by simulation models. The charge preparation at the sinter plant, returns handling, sinter conditioning and corresponding ventilation systems have been completely renewed. The annual smelting requirement is now achieved with two blast furnaces instead of three. This is the result of rebuilding and enlarging one of the furnaces and, of a completely new concept of the charge proportioning and charging systems, together with oxygen enrichment and blast air preheat. Ventilation capacity has also been drastically increased. A 7 MVA electric furnace for cleaning the slag from both blast furnaces. contributes to improving the overall metal recovery.

Jan 1, 1990