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By Wang Youlai

Sichuan province is the richest province for its waterpower resource in China, perfectly suited to develop a high consuming energy industry. Sichuan Aostar Group Company has two Aluminum smelters, Guangyuan Aostar smelter and Sichuan Aostar Smelter. The production capacity of Aostar Group was 240,000 tons in 2004. The construction scale of Sichuan Aostar Aluminum smelter is 250,000 tons per year. The first 168 GY-300KA pre-baked anode cells (125,000 tons/year) were put into production in 2003. This company has taken the lead in the use of the transfer gantry technology in China. Besides making the process of calibration the pot shell it has concentrated the efforts to construct cell lining elsewhere. This company also has taken the lead in China for using the EIRICH force mixing and cooling technology as well as in the world for the CP Company?s vertical ball mill technology that produces the pre-baked anodes. The carbon anode system completed its 190,000 tons/year production scale. This is the most advanced technology and the biggest scale pre-baking anode manufacture in China. Since the Sichuan Aostar 300KA cell was put into production, it runs normally and smoothly. Up to now the current efficiency is higher than 94% and the specific energy is only 13300kWh/T-Al.

Jan 1, 2006

By V. B. Chernyavsky, Ladokhin S. V.

Equipment and continuous casting technology for the production of small diameter copper rods and tubes are described. Industrial copper wastes, such as scrap and shavings, were used as the charge. An electron-beam installation for rod and tube production includes a crucible with an electromagnetic stirring system and a pouring hole in its bottom, a bottomless mold, .and a special cooling system, which includes an oil and water cooling devices. For the first time in the electron-beam technology, rods of 8 mm and 14 mm diameter mm tubes of 14 mm external diameter and 7 mm internal diameter were produced through continuous casting by pulling them out of the vacuum chamder into the atmosphere with depressurizing the vacuum chamber. The production capacity of a single strand continuous casting machine was 200 mm/tnin for rod casting and 150 mm/min for tube casting.

Jan 1, 2000

By Michael J. Virnig

The formation of crud is a normal part of operating a solvent extraction circuit for the recovery of copper. It periodically must be removed from the circuit. This results in significant costs in terms of manpower, downtime, and loss of circuit organic. Field studies have been carried out that show that the presence of a thermodynamic modifier in the organic phase contributes to crud formation. In an effort to better understand what factors contribute to crud formation, laboratory studies involving competitive adsorption studies with model solids have been carried out. The results of these laboratory studies will be integrated with the results of the field studies to present a better understanding of crud formation.

Jan 1, 1999

By C. Twigge-Molecey

All projects that are implemented, have been given corporate go-ahead on the basis of a set of clearly defined targets. These are typically a production goal at a capital cost, operating cost and production schedule, that will yield an acceptable return on investment by the companies internal criteria. The challenge for the implementation team is two-fold, firstly to properly define the project criteria prior to board approval and secondly to deliver an operating facility that meets these objectives, in particular the ROI. The paper addresses the issues a project team and the company management must address for a successful project. Key questions that will be explored are: ? What is the status of key technologies? Are they well proven in commercial practice, completely novel or in between? ? Is the project schedule driven by market constraints or cash flow constraints? ? Are the risks of fast tracking worth the potential rewards? ? For a retrofit project, are all the technical and production interfaces and issues known at the time of approval to proceed? ? How much should be invested in technological development and engineering and at which phase? ? For an owner-operator, how much responsibility is it wise or appropriate to push down to vendors? The answers to these questions for a specific project will define how you go about a project, the resources required, the contracting strategies, the phasing and the appropriate level of investment in the definition and procurement phases, prior to starting major capital commitments and construction.

Jan 1, 1999

By Alexandre Monteiro

Alumina precursor powders can be precipitated from aqueous solutions, using hydrothermal decomposition of urea to deliver base homogeneously to the system. Primary particles agglomerate early in the process, generating a wide size distribution. The presence of a polymeric surfactant such as polyacrylate can suppress or delay agglomeration, reducing particle size and narrowing the size distribution. The stabilization of commercially available a-Alp03 powder with polyacrylate was studied, investigating the effects of polyacrylate molecular weight, ionic strength and temperature. The effect of aluminum concentration, polyacrylate molecular weight and urea concentration on the precipitation of alumina precursors in a sulfate- urea system in the presence of polyacrylate/polyacrylic acid was then studied. The hydrolysis kinetics were followed, and particle sizes were determined. Precipitates were further characterized using energy dispersive spectroscopy. The particle characteristics are discussed in terms of the process conditions.

Jan 1, 1994

By Fatbardha Osmani, Skender Osmani

"A system analysis of the resource and environment management (water, energy etc) starts from its definition. Unfortunately, there is not a unique semantics of the mentioned concept. On these circumstances, in this paper the following issues are presented: 1.A short view on the existing concepts of management. 2.A new definition on the concept of management. It is considered as a complex and rational activity on human and natural resources ,environment etc, which starts from a analysis of infrastructure ,technology , etc, mission , alternatives , project etc. and ends to an optimal output. Basing on this definition, the management has two principal components: strategy and policy. The strategy is referred as a blue print program (the same definition as in Game Theory), which contains all the contingency alternatives. , while the policy is referred as a strategy applied into practice. The strategy is the first , while the policy is the second one. The best alternative of a policy is the project, Each strategy has one and only one project. The mentioned definition erases the differences between concept of policy and politics. Each strategy has its alternatives ,the next has its sub strategy and so on, i.e. whatever are going to be the strategy, there are a hierarchy composed by sub strategies up to the simplest strategies applied by a single individual (human beings or robots). The strategy objectives are necessary and sufficient conditions for its realization i.e . the strategy is an optimal activity, in which all resources are integrated and processed . Several strategies could be joined into one( for example the surface water strategies of the Balkan countries) . In this view, the strategy could be globalized into optimal way basing on different criteria’s as social, economic, environmental, their risks and effectiveness etc. etc An example from the water management illustrates the mentioned concepts."

Jan 1, 2008

By Vladimir Lobanov, Vladimir Skorohodov, Boris Radionov, Olga Makovskaya

"The synthetic sorbents and the activated carbons which are used for the metals extraction from weak process liquors are rather expensive. It is propose to use mineral and synthetic high-porous substances which sharply increased sorption properties by special processing. For achievement the desirable properties sorbents are impregnated by specially prepared solutions. Such solutions should contain the substances or its anionic forms which on the one hand are strong enough fixed in a supporter pores, with another are capable to form the insoluble compounds with extracting metals. Selectivity is provided by chemism of the reagent interactions with extracting metal. Due to the high concentration of a reacting ion in a sorbent phase the capacity and rate of sorption increases. Formed insoluble compound remains in a phase of the sorbent and necessity of its filtration disappears. For synthesis the sulfhydryl compounds which chemical properties allow to increase degree of extraction and capacity of the activated carbon were used. At hydrometallurgical processing of precious metals mineral raw materials the commercial solutions with the concentration of gold from 0,1 to 5 mg/dm3 are received. Commonly gold is precipitated from cyanic solutions by the zinc dust. The sorption methods are widely applicable. But the synthetic sorbents and the activated carbon using to these purposes are rather expensive. Expenses for sorbents even at its regeneration can reach 10-15 % from total expenses of gold extraction from ores. When sorbent regeneration, mostly for carbon, is not provided, this share increases to 30-40 %. Thereupon search of the sorbents combining availability, the sufficient capacity, demanded degree of extraction and the low price is actual. For the specified purpose it is offered to use the mineral and synthetic high-porous materials which sorption properties are sharply rose by special treatment. Among such substances are natural zeolites, silica gel, lignine et al. Similar treatment can improve the sorption properties of sorbents used in practice, particularly, the activated carbons. The simplest treatment of potential sorbents consists in its impregnation by specially prepared solutions. Such solutions should contain substances or its anionic forms - impregnating agents. These agents should be on the one hand strong enough fixed in a carrier pores, on the other hand are capable to form with extracting metals insoluble compounds. The more strong compounds are formed the high degree of metals extraction from solutions. The sorbents with similarly changed properties are named the impregnated sorbents."

Jan 1, 2008

By A. A. Bustos

Four Air Liquide Shrouded Injectors (ALSI ) were installed and operated for over one year in a Peirce-Smith converter at the Falconbridge nickel smelter in Falconbridge, Ontario, Canada. A shrouded injector consists of an inner pipe and an annulus, through which high oxygen enriched air and nitrogen flow, respectively The nitrogen cools the injector and protects the refractory in the vicinity of the injector tip, allowing for substantial increases in oxygen flow rates to the converting reactions. Several injector designs were tested to study the effect of changes in the cross-sectional area and changes in the entrance geometry of the annulus. An optimum design would minimize the injection pressure required for a given flow rate to achieve choked flow conditions at the tip of the injector. The operation of the ALSI was simple and did not require any special care or maintenance, either between blows or between converter cycles. In particular, the shrouded injectors did not require punching, as is the case with conventional tuyeres. In terms of refractory performance, the ALSI, operating at 30-40 % oxygen enrichment, were superior or equal to the conventional tuyeres, which operated at 21-23% oxygen. The results of the demonstration program led Falconbridge Limited to implement the ALSI technology on a commercial scale The paper presents the demonstration program results in terms of gas flow rates, accretion formation, punchless operation and refractory wear.

Jan 1, 1999

By S. K. Kawatra

"A typical steelmaking facility produced 50,000 tons per year of slag in their hot-metal desulfurization process. This slag had a sufficiently high iron content that it could be beneficiated and recycled in a blast furnace, provided that the slag could be agglomerated into pellets suitable for use as blast furnace feed. In this work, beneficiated slag was agglomerated using both a conventional bentonite binder, and a fly-ash-based binder (FBB) that was formulated by the investigators. The FBB consisted of a combination of highcarbon fly ash with calcium hydroxide activator, allowing the FBB to exhibit binding properties when moistened. It was determined that beneficiated slag agglomerated with FBB had superior compressive strengths compared to slag agglomerated with conventional bentonite binder. The FBB is therefore a satisfactory method of binding the agglomerated slag. Since the fly-ash component of the FBB is commonly discarded as waste, this approach also provides a means for utilizing high-carbon fly-ashes that currently have very little commercial value.IntroductionIn 2006 approximately 72.4 million short tons of fly-ash were produce in the United States [1]. The majority of fly-ash which was used that year was consumed concrete, structural fills, and cement. It is also used in road base, aggregate, and other applications. However, 55.2% of the fly-ash produced in 2006 was not utilized and ended up being sent to a landfill. Essentially all of the land filled fly-ash could be a suitable binder for pelletizing desulfurization slag and other steel plant waste oxide materials. Fly-ash based binders (FBB) have been shown in laboratory studies to be suitable for producing iron ore concentrate pellets of equivalent strengths as those bonded with bentonite [2,3,4]. The utilization of highcarbon fly-ash within the market is important for reducing the volume of currently unmarketable and land filled fly-ashes. FBB would be a much cheaper alternative to the current bentonite binder or organic binders used for iron ore concentrate and would help to reduce pellet costs. Currently, transportation more than doubles the final cost of bentonite since it is produced hundreds of miles from the pelletizing plants, while fly-ash is produced from power plants located nearby pellet plants and steel mills. FBB’s also show promise for use in other high volume applications such as foundry sand mold binders."

Jan 1, 2008

By B. Wan

The process of synthesizing silica nanopowder by the gas phase thermal oxidation of tetraethylorthosilicate (TEOS) in a diffusion flame reactor was simulated using a commercial computational fluid dynamic (CFD) code. The fuel combustion process and silica particle formation and growth in the flame are modeled. The temperature, velocity and particle size distribution (PSD) fields inside the reactor are computed. Chemical reaction rate and population balance model (PBM) were used to calculate the particle formation and growth and PSD.

Jan 1, 2006

By A. Robles

The main goal of the present work is to propose a viable alternative for selective arsenic elimination from copper smelter flue dust without the need of a global leaching scheme for all the individual components of the flue dust. Using this alternative, the inherent copper recovery problems are avoided. Arsenic precipitation is also considered for regenerating the solution and completing the process cycle. The experimental results for arsenic extraction and precipitation are satisfactory. Concentration of NaOH used was relatively low. The main reason for succeeding in high arsenic extraction and low NaOH consumption is due to the previous water washing of the flue dust. Water washing dissolves much of the iron and copper that are present in certain percentage as sulphate.

Jan 1, 1999

By Ennio Bonetti

The technological applications of MgH2 hydrides for hydrogen storage demand the overcoming of some critical issues: an improvement of the reaction kinetics and a reduction of the desorption temperature. The synthesis of nanocrystalline MgH2 by reactive milling and inert gas condensation and a proper metal catalyst addition, constitute recently employed strategies. In the investigation of the hydrogen short and long-range dynamics, sorption kinetics and nanostructure stability, the mechanical spectroscopy offers some specific advantages. In the present research this technique was employed with other experimental approaches (XRD DSC) to investigate relaxational and structural damping processes in nanocrystalline MgH2 with added catalysts (Fe). Time/temperature variation of the dynamic elasticity moduli and mechanical quality factor are correlated to hydrogen anelastic relaxation processes and concomitant structural transformation of MgH2 to Mg associated to long range H diffusion. Results are discussed with reference to microstructural modification strategies able to assist hydrogen release.

Jan 1, 2006

By Kurt Svens

"As zinc consumption is gradually increasing all the time in the world, many zinc plants are looking for possible expansions. As the sulphuric acid market as well as the fertilizer market in many areas is saturated, the costs for the roasting-acid plant section of the zinc plant will create problems when making feasibility calculations for possible expansions. For solving the customers' situation, two proven zinc concentrate direct leaching technologies are available. A third one, which is possible, does not have any industrially proven applications in the zinc area.IntroductionTime to time, the zinc plants in the world scrutinize their operations with respect to their cost efficiency, the total zinc recovery and the near-by or far-away consumer markets, especially the for zinc and sulphuric acid. Their preliminary profitability calculations can show that a possible total expansion is not economical, when they are looking to expand the whole roasting/acid plant - leaching - solution purification - electrowinning - casting route, as the possible market price for the sulphuric acid is low or the sulphuric acid market is too far away. Based on these facts, their economical study often indicates that implementing a zinc concentrate direct leaching option could be more favourable. Regarding this situation, several aspects concerning three alternative direct leaching methods will be discussed, of which pressure leaching and the atmospheric leaching processes have several industrial applications in the zinc industry, as the ultrafine grinding - conventional leaching process at present has none. As iron is also dissolved during zinc concentrate direct leaching, iron removal processes generally used in the zinc industry are additionally discussed below."

Jan 1, 2012

By David J. Krichten

A method of retrofitting air-fuel burners with oxy-fuel capability overcomes the potential problems associated with oxygen combustion in aluminum melting furnaces. The retrofit burner uses the existing combustion air connection, burner housing, and burner tile and replaces the gas tube with an oxy-gas burner. Maintaining a portion of the air flow to the burner reduces the potential for localized overheating. Proper design of the burner reduces NOx emissions by moderating the flame temperature with furnace gas recirculation. Economic analysis of using oxygen shows the benefits are increased productivity and reduced overall unit cost of melting. In practice, the melt rate in rotary furnaces increases by up to 50% and by up to 35% in reverberatory furnaces. Oxygen utilization reduces total melting cost by 112-314 cents per pound of aluminum melted.

Jan 1, 1997

By Olli Järvinen

The capacity of the Outokumpu Pori refinery is today about 125 000 mt in 1998. The anode slime amount is about 700-800 mt. The copper is removed with pressure leaching. Selenium roasting is done with the gas roasting. The doré smelting in the furnace is done with the tilting rotating converter with oxy-fuel burner (TROP). Doré anodes are treated in the silver electrolysis. Gold is recovered from the gold mud with the quick hydrochloric acid leaching process. The important point in the leaching is to get into contact the solid copper with the oxygen and liquid. Outokumpu has an efficient agitator for this purpose. The GLS-agitator (GLS=gas, liquid and solid) is powerful for mixing oxygen, liquid and solid together. The current production in Pori plant is 40000 kg of silver, 5000 kg gold, 40000 kg of selenium and one hundred kilograms of platinum-palladium concentrate.

Jan 1, 2000

By Bob Drew, Alfred Spanring, Kirschen. Marcus

"Increasing material conversion and energy efficiency, and decreasing carbon dioxide emission levels are crucial for sustainable production processes in the aluminum, cooper, and steel industries. RHI supports these targets by providing a diverse range of solutions including high quality refractory linings, optimum lining maintenance, and process improvements. In this paper examples are provided of process improvements and increased energy efficiency in copper refining, potential energy savings during electric arc furnace and ladle operations in the steel industry, and increased energy efficiency by improved heat transfer in anode baking furnaces in the aluminum industry. In all cases, RHI’s expertise in close collaboration with the customer resulted in an improved performance of the reactor lining and the actual high temperature process with a positive impact on the material conversion and energy efficiency and as a result a decrease in specific carbon dioxide emission levels.IntroductionRefractory linings play an important role in heat transfer during high temperature processes in for example the aluminum, copper, and steel production industries. Due to constantly increasing energy prices worldwide and the increasing demands for environmental and climate protection, improving the energy efficiency and decreasing emission levels of these energy intensive production processes is of significant importance. In this paper, the contribution of modern RHI lining technologies to energy saving measures and the corresponding reduction of specific carbon dioxide emission are described. The type of current refractory solutions for energy intense processes are illustrated with four examples: Optimization and increase of material conversion and energy efficiency in copper refining, energy saving potentials in both electric arc furnace and transport ladle operations in the steel industry, and heat transfer improvements during the carbon anode annealing process in the aluminum industry. These examples focus on particular production processes operating with a high proportion of recycled copper, steel, and carbon anodes. Increased energy efficiency directly decreases the specific energy related carbon emission levels whereas improvements to the metallurgical processes aim to increase material conversion efficiency and, therefore, decrease specific process related carbon emission levels. Significant energy savings can be achieved by maximizing the refractory campaign length through a combination of appropriate refractory material selection, grade zoning, correct installation, careful preheating, and effective maintenance strategies. Besides the efforts to improve the performance and energy efficiency of customer high temperature processes, RHI continuously promotes the development of new low emission carbon-containing refractory bricks and unshaped products."

Jan 1, 2008

By Jean Igor Margem, Rômulo Loiola, Sergio N. Monteiro, Foluke S. de Assis, Frederico M. Margem

"Fibers extracted from the ramie plant have been traditionally used in textile and are now being considered as polymeric composite reinforcement owing to their superior strength. Recently the mechanical behavior of ramie fiber reinforced polyester composites was investigated but no significant improvement was found. Therefore, the objective of this work was to carry out a similar investigation by changing the type of polymeric matrix. Specimens with up to 30% in volume of ramie fibers incorporated into epoxy were bend-tested until fracture. The results showed a moderate improvement with a tendency of decreasing stress for higher amounts of ramie fibers due to the weak interface developed with the epoxy matrix.IntroductionThe engineering application of natural fibers extracted from cellulose-containing vegetables, also recognized as lignocellulosic fibers, is presently considered an environmentally correct alternative to replace more expensive, non recyclable and energy-intensive synthetic fibers [1-3]. In fact, composites reinforced with traditional fibers such as coconut, sisal, jute, hemp, etc ... are already on the market in substitution for common glass fiber automobile components [4-6]. Even less known fibers like curaua from the Amazon region are being industrially used [7]. Economical and environmental reasons sustain a promising future trend for natural fiber composites. In comparison with the less expensive glass fiber among energy-intensive synthetics, lignocellulosic fibers are approximately five times cheaper. For the current situation of our planet, natural fibers are regarded as ""green"" environmentally friendly materials. They are abundant, renewable, biodegradable, and recyclable, above all, neutral with respect to carbon dioxide emission, associated with global warming.Several relatively unknown lignocellulosic fibers such as piassava [8], sponge gourd [9], sugar cane bagasse [10], buriti [11] and ramie [12], with simple and limited applications, or just byproducts, are now being investigated for their potential as composite reinforcement. This could widen the offer of new lignocellulosic fibers for composite reinforcement. The banana fiber, in particular, has a tensile strength around 700 MPa [13], which is comparable to the strongest lignocellulosic fibers used as composite reinforcement.In addition to polyester, the epoxy is another relatively strong polymer used as composite matrix. Therefore, the objective of the present work was to assess the mechanical properties obtained by flexural test, for epoxy composites reinforced with different amounts of banana fibers."

Jan 1, 2013

By Shadia J. Ikhmayies

"Cadmium sulfide (CdS) in the form of thin films is an interesting material because it has a large variety of applications ranging from photovoltaic to luminescent devices. N-type CdS is usually used as a window layer in the heterojunction CdS/CdTe thin film solar cells. A review of the photoluminescence (PL) spectra ofn-type CdS thin films prepared by different techniques was performed. The effects of different dopants and impurities and the effects of temperature and deposition parameters on the PL spectra were discussed. Annealing in different atmospheres causes the changes in material structure and phase change from cubic to hexagonal phase which can be detected through the variations in the PL spectra. CdCh heat treatment improves the cystallinity of the films and enhances the exciton peaks and the green band in the PL spectra.IntroductionThin CdS films deserve attention because their expected gap emission lies very close to the highest sensitivity of the human eye. Thus, one might assume that thin CdS films are an appealing host for photonic devices [ l]. They have been used in a lot of applications including electronic and optoelectronic devices [2]. Thin films ofn-type CdS are widely used as a window layer in heterojunction solar cells such as CdS/CdTe solar cells. Doped and undoped CdS thin films can be obtained by different techniques such as; spray pyrolysis (SP) [3], chemical bath deposition (CBD) [2, 4], pulsed laser deposition [5, 6, 7], laser ablation [l], thermal evaporation [8].Several experimental techniques have been used in order to study semiconductor defects. In particular, photoluminescence (PL) has been shown as a powerful and sensitive tool in examining the crystal quality of polycrystalline thin films. PL can be used in the detection of defects which are radiative active. These defects can also act as traps in the transport of carriers [9]. The photoluminescence (PL) of thin film CdS is strongly influenced by the unbalanced stoichiometry, which is typical for CdS and is in general evoked by a Cd surplus. With increasing Cd content, the emission spectra move far below the gap to the red spectral range. Besides stoichiometry problems, independent of the material deposited, the PL properties of thin films depend on surface features and the influence of the interface between the film material and the substrate [10]."

Jan 1, 2013

By D. F. Liub, Z. Y. Liu, W. Y. Xue, Y. F. Shenb, Y. D. Wang

"The microstructure characteristics and deformation behavior of ultrafme grained (UFO) 304SS fabricated by accumulative rolling and armealing have been investigated by means of tensile tests, electron-backscatter-diffraction (EBSD) and transmission electron microscopy (TEM) techniques. The volume fraction of martensite phase decreases with increasing armealing temperature. In the grain sizes ranging from 300 nm to 10 µm, the strength held Hall-Petch relationship. The sample with an average grain size of 300 nm exhibited extra high yield strength of 1700 MPa and a tensile strength of 1780 MPa, while the elongation retains 12%. The limited uniform elongation in the UFO materials could be explained in terms of plastic instability. Very interestingly, for the bulk material with an average grain size of 1.200 µm, the high yield strength and uniform elongation were simultaneously achieved to be as 1000 MPa and 18%, respectively.IntroductionUltra-high strengths have been achieved in elemental metals by employing heavy plastic deformation, or by creating ultra-fine-grained (UFO) structure. Here UFO materials are defined as polycrystalline solids with property-controlling microstructural features below the 1 µm level. Typical processing routes include severe plastic deformation (SPD) [1, 2], which decomposes the grains through dislocation accumulation and reorganization (polygonization). Several different kinds of SPD process for bulk materials are typically as equal-charmel angular pressing (ECAP) [3], high-pressure torsion (HPT) [4] and accumulative roll-bonding (ARB) [5]. One of the main motivations for such a push for the very small grain sizes stems from the expectation of unprecedented mechanical strength, as predicted by the well-known Hall-Petch relationship that projects a continuous rise of strength with decreasing grain size [6]. However, these ultra-high strength metals no longer have the high ductility typical of their conventional coarse-grained counterparts, because the undesirable inhomogeneous deformation on the microstructure level can lead to the early onset of failure, severely limiting the useful ductility [2]. Recently, the interesting strategies have been performed to increasing simultaneously the ductility and strength ofUFG pure copper and nanostructured alloys by Zhao et al [7, 8]. In a pure copper, a high ductility has been achieved without sacrificing strength by introducing a high density of pre-existing twins and a large fraction of high-angle grain boundaries. Their encouraging results trigger our motivation to obtain high strength and ductility from the commercially bulk material."

Jan 1, 2013

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