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By Adam Gesing, Paul Marchwica, Jerry Sokolowski, Sharon Lackie

"Often referred to as SEM-EDX, energy-dispersive spectroscopic analysis of characteristic fluorescence x-ray is a standard technique for semi-quantitative elemental composition analysis in scanning electron microscopy. It is quick and extremely useful for identification of phases in the sample microstructure, as long as the constituents are significantly larger than the probe volume from which the fluorescence x-rays originate. The probe volume ranges from a few to several microns, depending on the electron beam spot size and the acceleration voltage. We report on a new variant of an EDX technique developed to overcome this limitation and allow quantitative elemental analysis of smaller phase constituents, down to a size of several nanometers. This variant involves the calculation of compositions of individual phases from multiple analyses of areas containing phases of interest. This significantly increases the usefulness of EDX for quantitative analysis of new nano-structured materials.IntroductionIn any elemental micro-analytical method, the sample material is illuminated by a probe beam that excites an interaction volume of a sample to emit a characteristic signal. This signal in turn interacts with the sample material through absorption and fluorescence mechanisms before a portion of it is collected by a suitable detector and analyzed for elemental composition. The spatial resolution of the method depends on the minimum interaction volume between the probe beam and the sample material.Laser light beams can be tightly focused to a spot size limited by the photon wavelength and can be used to sample the surface of any material. In micro-LIBS (laser-induced plasma spectroscopy) a focused laser beam ablates and vaporizes a small volume of material from the sample surface, creating a plasma spark. Spectral analysis of the light emission from the plasma spark allows the semi-quantitative determination of the elemental composition of the material removed from the sample surface. The smallest reproducible craters achieved are ~ 3mm in diameter and a few nanometers in depth. [l]Particle probe beams of ions or electrons can be focused to a diameter of a few nanometers at the point of impact on the sample. Ions sputter the sample atoms from the point of impact, and the sputtered ionized material is analyzed by mass spectroscopy in a secondary ion mass spectrometer (SIMS). [2] This gives SIMS resolution in a nanometer range. SIMS equipment, however, is expensive and not readily available."

Jan 1, 2013

By Pinakin C. Chaubal

Today?s steel industry is in a vibrant and resurgent mode. This transformation has been in the making for some time now. Over the last few decades, the industry was steadily transforming itself into becoming a high tech industry. New technology was adopted, efficiencies were enhanced, lean manufacturing concepts were brought in and a strong customer focus was developed. Today?s mills employ sophisticated instrumentation, computerized monitoring, on-line smart systems etc. driving processes that are producing at rates of many tons/minute. All this is not possible without judiciously using the latest available technologies in various fields and developing a more sophisticated work force. Prof. Sohn has been a pioneer in driving the concept of process engineering in process metallurgy. In this paper the focus is on some aspects of process engineering ? primarily process modeling - as applied to iron and steelmaking processes. Examples are shown to demonstrate how problems have been addressed. Some thoughts on future directions are presented.

Jan 1, 2006

By G. C. Yao

Branch and needle-shaped intermetallic compounds of iron, silicon and aluminum normally exist in the molten aluminum. If a suitable amount of manganese metal is added into molten aluminum, the shape of the intermallic compound particles may become lumpish and spherical. According to the difference in electric and magnetic properties of these impurity particles and molten aluminum, these impurity intermetallic compound particles can be separated by applying an alternating magnetic field. In this experiment the alternating magnetic field was formed by a "c" type loop with AC (50Hz) current. The inner vacuum of the fireclay refractory separator is 25xl5xl30mm3 with a lateral baffle inside. The separator was put into the interspace of the "c" type loop. It was found that the longer the separation time, the larger the amount transferred of impurities. The amount of transferred impurities increases with the increase of separation time and intensity of magnetic field. The addition of manganese metal enhances significantly the efficiency of impurity separation

Jan 1, 2003

By L. Filip

The roast-leach-electrowinning (RLE) process for zinc was modified to treat two typical complex concentrates containing zinc, lead, copper, gold and silver. Laboratory testwork results indicated that the optimum roasting temperature ranged from 700 to 800°C, in order to produce acceptable residual sulfur levels. The calcined concentrate was subjected to a three-stage leach sequence. The resulting leach solution was purified by hematitic precipitation and directed to the recovery of copper and zinc by solvent extraction and electrolysis. Alkaline smelting and subsequent electrolytic purification recovered the lead and precious metals from the leach residue. A flowsheet was developed based on the laboratory testwork results, and demonstrated in a large-scale pilot plant. The recoveries produced during the pilot plant operation ranged from 90 to 92% for zinc and copper, 85% for lead and 90% for gold and silver, respectively.

Jan 1, 1999

By I. H. Gundiler

Sandia National Laboratories (SNL) is tasked to support The Department of Energy in the dismantlement and disposal of SNL designed weapon components. These components are sealed in a potting compound, and contain heavy metals, explosive, radioactive, and toxic materials. SNL developed a process to identify and remove the hazardous sub-components utilizing real-time radiography and abrasive water-jet cutting. The components were then crushed, granulated, screened, and separated into an aluminum and a precious-and-base-metals fraction using air-tables. Plastics were further cleaned for disposal as non-hazardous waste. New Mexico Bureau of Mines & Mineral Resources assisted SNL in investigation of size- reduction and separation technologies.

Jan 1, 1995

By I. D. Reznik

Results of thermodynamic computations have been presented for reactions occurring in the process of segregation roasting of oxide nickel ores to describe more accurately the mechanism of the process. Under conditions of laboratory-scale roasting in combination with close-circuit flotation flow-sheets and magnetic separation, a recovery of 80-82% of nickel into 8 to 10% Ni concentrate and a recovery of up to 66% of cobalt was achieved. Process conditions have been selected for processing of both high-iron and high-magnesium ores. The feasibility of conversion of 94-98% of nickel and cobalt into solution by oxidizing pressure leaching with sulfuric acid has been demonstrated. It has been substantiated that it is reasonable to introduce double-stage segregation roasting.

Jan 1, 2003

By P. Koskinen

Outokumpu Oy has 30 years' experience in nickel production. It is mainly based on the technology developed within the company. The production chain starts from the mines reaching to the high-grade cathode nickel and the stainless steel manufacturing. As a multi-metal producer Outokumpu has the advantage to exploit from nickel raw materials also other valuable metals and intermediate products which can be processed at the company's various plants. The main source of nickel concentrate is nowadays the Enonkoski Mine started up in early 1986. It is the most modern mine in Finland being provided with the latest Finnish high-tech systems. Nickel concentrates are smelted at the Harjavalta Works using Outokumpu's internationally well-known flash smelting method. Also nickel containing residues and secondaries' are used as raw materials. The high-grade nickel matte from the smelter is then refined at the nickel refinery in a hydrometallurgical process, which was also developed by the company's own research staff. These processes have been continually improved and capacities gradually enlarged to 18 000 mtpy of cathode nickel. Besides plating, melting and superalloying purposes part of the nickel ends in stainless steel at the Tornio Works. The production was started in 1976 and has reached an established position on the European market.

Jan 1, 1988

By Dajian Wang

To obtain the thermodynamic properties of a multicomponent liquid alloy system over the whole range of concentration at an arbitrary temperature, the free volume cell theory has been applied to derive the formula of activity coefficients of liquid solutions based on the infinitely dilute solutions at some temperature. The linear logarithmic relationship between activity coefficients of binary dilute solutions and reciprocal of absolute temperature have been verified, and are in good agreement with the experimental values from the literature. The Monte-Carlo algorithm was used to calculate the nonlinear end value equations of binary systems, then the free volume parameters obtained were correlated with the activity coefficients of liquid binary, ternary, and quaternary systems at an arbitrary temperature. Three dimensional a-X-T diagrams of some binary systems representing the temperature and concentration dependence of activities were plotted. The calculated results regarding non-ferrous alloy systems have been statistically examined with the experimental values from the literature. Hence, this simple approach could be useful for analyzing thermodynamic properties of liquid alloy systems.

Jan 1, 2000

By S. C. Grund

In secondary copper smelting as it is performed at Hüttenwerke Kayser plant in Lünen, tin-and lead-containing flue dusts are produced as intermediate products. These flue dusts are further processed in a hearth furnace. Followed by certain refining operations a saleable tin-lead-alloy is produced. Even though the hearth furnace technology has been in use for this purpose for a long time still its performance undergoes changes in search for optimum processing conditions regarding to the increasing complexity of the raw materials and tightening economical and ecological boundaries. The use of modern statistical tools for the calculation of accurate mass balances is demonstrated for the tin-lead hearth furnace. These reliable mass balances are the basis for any further modelling of the process with the aim of optimization. Incorporating metallurgical knowledge and experience as well as different mathematical modelling techniques, further studies are planned in which the recoveries of valuable and minor elements and their dependency from various process parameters are examined. The aim of this modelling is to optimize the recoveries of the valuable elements, to minimize the energy consumption and the processing costs and thus to keep the process competitive in a harsher economical and ecological surrounding. The modelling principles are transferable to other metallurgical operations and are especially suited for ill-defined pyrometallurgical processes.

Jan 1, 1999

By V. I. Lakshmanan

"Historically flowsheets are developed for efficient separation of metals for economic recovery. With increasing emphasis on reduction, reuse and recycle (3Rs) efficient methods are sought to recover values from a variety of feeds where cost of collection, transportation, local consumer behaviour and regulatory guidelines dictate the development of economically viable flowsheets. Innovative understanding of potential market applications can provide means to develop value added end products. The paper with examples will discuss the use of innovative-separation technologies to obtain value added end use materials from secondary sources.IntroductionFlowsheets are developed for the efficient separation of materials of value for economic recovery. However with increasing societal pressures and regulatory initiatives for stricter environmental guidelines, there is strong need to provide focus to recover materials efficiently and economically in an environmentally accepted manner. North American industries are increasingly caught between demands for high technology value added products and responsibility for environment. An aspect that is receiving increasing attention is Design for Environment'. This incorporates a system wide approach for product design and incorporates environmentally preferable features such as recyclability, disassembly, maintainability, reusability and use of safe materials as part of a product's design objectives.The present paper with case histories will address innovative flowsheet development to convert wastes into recyclables value added products or for minimising generation of waste materials. Case HistoriesProcess for Separating Fibres from Composite Materials 1In the automotive industry, sheet molded compound (SMC) is used to produce panels, bumpers and the like. During the manufacture and at the end of life, considerable waste materials are generated which are potentially recyclable. Fibre reinforced plastics where fibre substrate impregnated with thermosetting resin, find applications in several manufacturing processes and are potentially recyclable at the end of life."

Jan 1, 1996

By Guo Xueyi

The environmental impact assessment of the Imperial Smelting Process for metallic zinc and lead production in Shaoguan Smelter, China, was carried out by the life cycle assessment method. The detailed inventory analysis of the Input/Output in the process during 1998-2000 was conducted and the allocation was done among the main products of zinc, lead and sulfuric acid, according to the system expansion and substitution principle, The environmental impacts were assessed by using the following five Eco-indicators: Gross Energy Requirement (GER), Global Warming Potential (GWP), Acidification Potential (AP), Heavy Metal Toxicity (HMT) and Solid Waste Burden (SWB). The results from this study are useful to address the environmental situation of the technology practice in this smelter, and provide a scientific basis for the further improvement.

Jan 1, 2003

By Fuqiang Zheng, Yufeng Guo, Pengfei Li, Guanzhou Qiu, Tao Jiang, Andrew Yakovlevich Travyanov

Low content of TiO2 and high impurities content of Ca and Mg are the shortcomings of domestic ilmenite. To meet the requirements of the material in the titania produced by chlorination process and titanium sponge industry, enrichment of ilmenite is necessary. In the process of enriching ilmenite, high temperature and reductive condition were beneficial to the formation of anosovite, but the high content of magnesium oxide which was solid soluble in anosovite baffled the following separation. So the effects of pre-oxidation and reductive conditions including reduction temperature, reduction time and hydrogen concentration on the phase composition and metallization rate were studied. The characteristics of reduction samples were analyzed by X-ray diffraction and optical microscope. Results have shown that the reduction product is mainly composed of Fe, Fe(Mg)TiO3 and TiO2 at 1123K, its metallization rate is about 65%,magnesium exists in Fe(Mg)TiO3.

Jan 1, 2015

By R. E. Brewer

Pilot scale flotation tests were conducted with a l?ft-diam column at the Barrick Resources (USA) Mercur mine, Tooele County, UT, to scavenge unleached (0.01 to 0.018 oz/st) gold values from the tailings of a carbon-in-leach (CIL) circuit. The optimal recovery was 35 pct of the unamenable-to-leaching gold, at a grade of 0.353 ounces of gold per short ton, using a mixture of dithiophosphate, xanthate, and diesel fuel as a collector. This was achieved by floating approximately 1.6 wt pet of the CIL tailings. The gold values are believed to be contained in arsenic-bearing minerals, attrited carbon, and carbonaceous material in the ore. Redox potentials were measured with a gold electrode during the conditioning stage prior to flotation. The correlation between flotation recovery and redox potential values could be used to control reagent additions. Treatment of a previously leached and weathered tailings material, averaging about 0.055 ounces of gold per short ton, was also investigated. The tailings were first water leached at approximately 60? C, and the water-leached tailings, containing approximately 0.03 ounces of gold per short ton, were then fed to the column flotation unit. The effects of pH' and sodium sulfide addition on gold flotation recovery and redox potentials were examined. Maximum gold flotation recovery, 36 pct, was achieved at pH 8,5 with a sodium sulfide addition of 0.18 Ib/st. Overall gold recovery by leaching and flotation was in the range of 70 to 80 pet.

Jan 1, 1989

By Sarah Beutner Mavrogenes

The mineralogy of three slags from a domestic secondary copper refinery were studied by applied mineralogical techniques to determine the: 1) phases present, 2) phase chemistry, 3) phase abundance, 4) associations, 5) crystalline habit, 6) grain size, 7)microtextures, and 8) causes for certain metallurgical problems, such as metal losses to the slags. The slags were produced by skimming the bath prior to melt-down to allow heat from the flame to reach the bath. The first slag is highly viscous and all three slags contain a large amount of copper. The "first slag", which is skimmed prior to treatment of the bath with fluxes, contains metallic copper, cuprite, delafossite, magnetite, Mg-hercynite, common spinel-chromite solid solution, picrochromite-chromite solid solution, common spinel-picrochromite solid soiution, gahnite, cassiterite, silica-rich glass, and corundum. Its abundant solid refractory phases make the slag difficult to skim. The "soda-rich slag", skimmed after the treatment of the bath with sodium carbonate flux, contains cuprite, delafossite, magnetite, cassiterite, Na-Al-silicate, and Na-Al-Ca-silicate. It contains less metallic copper than the first slag and lacks the refractory minerals. The "phosphorus-rich slag", skimmed after treatment of the bath with a copper phosphide flUX, contains metallic copper, cuprite, delafossite, berlinite, cassiterite, silica, apatite, Cu-Fe-rich apatite, copper phosphate, Cu-Fe-phosphate, and a Pb-phosphate. In contrast to the above three copper-rich slags, recent charges have produced a silver-copper-rich slag. The "silver-rich slag", skimmed after the treatment of the bath with a copper phosphor ide-borax flux, contains, cassiterite, delafossite, cuprite, a Na-Al-silicate, magnetite, metallic copper, MgO, common spinel-chromite solid solution, and wollastonite. Silver ranging from 0.05 to 2.02% was found by atomic absorption and inductively coupled plasma spectrometry analyses in the metallic copper phase.

Jan 1, 1989

By Kumar M. Lyer

The channel reactor for ferrous and nonferrous processing has been modeled as a combination of ideal reactors. Cold model studies simulated the counter-current flow of slag and matte (or metal) with high-strength submerged gas injection. A composite model has been developed which describes the mass transfer between the two liquid phases, including the transfer of minor elements. The residence time for the matte droplets in the matte/slag emulsion is compared with the settling rates for the matte droplets in the slag to determine their relative importance in the mass transfer between matte and slag. The governing equations for mass transfer have been developed using correlations for the mass-transfer coefficients in the continuous and dispersed phases. An application of this scheme to a typical copper smelting system is presented.

Jan 1, 1993

By J. F. White

An experimental study was undertaken to evaluate the feasibility of a selective chloridizing roasting pre?treatment process for the elimination of impurities from zinc feed?stocks prior to recovering zinc by conventional unit operations. In this investigation, a number of chemistries that might serve as a basis for such a pre? treatment process were examined. A variety of chloridizing agents were admixed with EAF dust to promote the selective removal of lead and cadmium by the formation of volatile metal chlorides, he results of the experimentation firmly establish that selective chloridizing roasting is a technically feasible means of eliminating lead and cadmium from EAF dust. Excellent extraction efficiencies were accomplished with a number of chloride additives; as high as 98 percent lead extraction and 88 percent cadmium extraction were attained with minimal zinc losses, Continuous pilot?scale tests reinforced the trends established by laboratory?scale experimentation, Attempts of chlorine elimination using pyrohydrolysis were less successful. The extent of chlorine elimination was found to be highly dependent upon EAF dust sample type and treatment temperature.

Jan 1, 1996

By H. Senoh

For the purpose of clarifying the reason caused a drastic decrease of discharge capacity for MmNi3.6Mn0.4Al0.3Co0.7 electrode at relatively low temperatures, various factors influencing the charge-discharge processes were investigated in the temperature range of 25°C to -40°C. The charge efficiency obviously decreased at low temperatures less than 0°C due to a decrease in the rate of the charge-transfer reaction on the electrode surface. Moreover, both the rate of the hydrogen diffusion from the alloy bulk to surface and the rate of the charge-transfer reaction significantly influenced the high-rate dischargeability. The addition of Mo to MmNi3.6Mn0.4Al0.3Co0.7 alloy was found to be effective for improving the electrocatalytic activity, leading to the improvements of the charge efficiency and the high-rate dischargeability at relatively low temperatures.

Jan 1, 2002

By Douglas K. Modrow

In the fall of 1993, construction was completed on a state of the art industrial waste water treatment plant at Asarco's East Helena Lead Smelter. Purpose of the plant was to remove arsenic and metals using hydroxide precipitation. Completing of the plant culminated a lengthy process of laboratory bench-scale test work, engineering, construction, and Environmental Protection Agency (EPA) oversight. Unfortunately, the effiuent requirements for the plant were made significantly more stringent as construction was rearing completion. As a result, optimization activities were initiated to determine and implement measures to substantially improve effiuent quality so the new discharge limits could be met. These activities consisted of acquiring a thorough understanding of process chemistry and plant operations, and developing simple, practical methods of automating unit operations associated with the treatment plant. Implementation of these modifications in the second half of 1996 will not only significantly improve the constancy and reliability of treatment plant operations, but also result in operating cost savings and reduced need for increased operator attention at capacity flows, plus allow the treatment plant to meet the new discharge limits.

Jan 1, 1996

By Chu Yong Cheng

Manganese is one of the main impurities in the recovery of base metals from their ores. This is especially true when laterite ores are processed using the pressure acid leach (PAL) process. The use of intermediate precipitation, solids/liquid separation and re-leach in the three Western Australian nickel laterite plants to separate nickel and cobalt from manganese and other impurities makes these processes complicated and costly in capital and operation. The research work carried out by the solvent extraction (SX) group at the A J Parker Cooperative Research Centre for Hydrometallurgy (CSIRO Minerals) has led to the development of direct solvent extraction processes to separate nickel and cobalt from manganese and other impurities. The simplicity of the process flowsheets and the expected savings in capital and operating costs are the major advantages of the new direct solvent extraction processes over the existing processes. By using a new synergistic organic system, Versatic 10 / dccyl-4-pyridinccarboxylatc ester, with a pilot plant leach solution from BHP¬Billiton (after iron precipitation), the metal values (Ni and Co) together with zinc and copper were separated from manganese and other major impurities (Mg, Ca and Cl) in the first SX circuit. The co-extracted manganese, magnesium and calcium were easily scrubbed out. The extraction and stripping kinetics of the metals with the new synergistic organic system were very fast and the synergistic system was found to be chemically stable. pH-extraction isotherms of metals with D2EHPA showed that the extraction order as a function of pH50 was Zn2+ > Ca2+ > Mn2+ > Cu2+ > Co2+> Ni2+> Mg2+. Semi-continuous test work with a cobalt pilot plant leach solution from Peko Rehabilitation Project Pty Ltd and a synthetic solution to simulate a concentrated laterite leach solution from BHP-Billiton showed that manganese, together with calcium, copper and zinc can be separated from nickel, cobalt and magnesium. This led to the development of another direct solvent extraction process to separate manganese and other impurities from nickel and cobalt and to recover nickel and cobalt from leach solutions. A project was initiated by HiTec Energy Ltd to recover manganese from waste laterite leach solutions using SX technology and to further purify it to produce high purity electrolytic manganese dioxide (EMD) for the high quality alkaline battery industry. Batch tests were conducted to select a suitable organic system for the extraction of manganese in terms of selectivity and extraction and stripping kinetics. A total of eight organic systems were tested using waste laterite processing solutions. A Versatie 10 / synergist system showed very promising results. By using the synergistic system, high manganese recovery would be obtained, fewer SX stages would be required and a higher A:O ratio could be used in extraction, resulting in a smaller organic inventory and lower capital costs. The risk of gypsum formation is also minimised with the synergistic system. Keywords: Solvent Extraction, Manganese, Laterite, Synergist

Jan 1, 2004

By Olusegun J. Ilegbusi

"A two-fluid model is used to calculate flow and heat transfer characteristics of a plasma jet. This model accounts for both gradient-diffusion mixing and unmixing that may result from pressure-gradient-body-force imbalance in the system. The unmixedness is considered to be essentially a Rayleigh-Taylor kind instability. Separate transport equations are solved for the plasma and ambient gas velocities, temperatures and volume fractions. The two fluids allowed to exchange mass, momentum and energy through empirical interaction parameters. The empirical coefficients are first established by comparison of predictions with available experimental data for shear flows. The model is then applied to an Argon plasma jet ejecting into stagnant air. The predicted results show the significant build-up of unmixed air within the plasma gas, even relatively far downstream of the plasma torch. By adjusting the inlet condition, the model adequately reproduces the available experimental data on the temperature profile.IntroductionPlasma jets have important applications in materials processing, some of which include spray deposition, melting and refining, heat treatment and materials synthesis. In a typical reactor, the hot plasma stream entrains a surrounding gas and the resulting heat and mass transfer and the condition of operation of the torch, determines to a large extent, the performance of the unit. The entrainment may prevent uniform mixing and produce regions of unmixed hot/cold gases and non-uniform deposits as a result of insufficient melting of deposit in cold regions. This phenomenon may also affect chemical reaction rate in plasma systems for NOx reduction in exhaust gases.The study of plasma phenomena is often conveniently divided into three parts namely, the plasma torch, the plasma jet and analysis of the particles carried in the jet. The present work concerns processes occuring in the near-field of the plasma jet i.e. just downstream of the torch."

Jan 1, 1994