Search Documents

In accordance with the new concept described in the paper presented at the TMS annual meeting in 1989, 1 a new zinc cellhouse was constructed and successfully operated. The new concept was proposed in order to reduce energy requirements and to mechanize the electrode handling in the cellhouse. Major modifications involved the use of an electrode unit consistfog of assembled anodes and cathodes with frame bodies between each cathode and anode. The space between a cathode and an anode could be halved by this unit structure. In this paper actual operation data are summarized and discussed in comparison with the calculated figures.

Jan 1, 1990

By Adrien Antenen, Didier Villette

CITRON has developed a new process for the recycling of hydroxide sludge, household batteries, catalysts, automobile shredding residues, grinding sludge and other metal containing organic and inorganic waste. A pilot plant with a capacity of 1,000 tons per year has started operations in April 1998. In August 1999, an industrial plant became operational with an initial treatment capacity of 23,000 tons.

Jan 1, 2000

By Rolando Campos

In August 1993, the operation of Refimet Chile's copper custom smelter commenced at La Negra, near Antofagasta in northern Chile. Design smelter throughput corresponded to 235 000 tonnes of concentrate, calcines and copper cements arising from suppliers in the north of the country to produce 90 000 t/y of blister copper. Refimet had initially gained experienced in building and operating leaching, roasting and a blast furnace facility at Rungue, near Santiago, followed by Roasting at La Negra. The initial smelter project was based on conventional reverb- smelting and Peirce-Smith converting and the majority of equipment was 'purchased second-hand and rehabilitated or modified. After only 3 years in production, the treatment capacity was significantly improved by introduction of technical improvements to the original plant operating scheme. Recently, the plant was further expanded to an annual smelting capacity in excess of 400 000 t/y feed, corresponding to around 160 000 t/y copper production. This expansion, referred to as Phase 2, was achieved by modification of the reverb to oxy-fuel firing, addition of a further (second-hand) acid plant, fire refining and anode casting facilities. Parallel development of concentrate injection into enlarged converters-also took place. Following successful commissioning of Phase 2 expansion, initial engineering studies for a third expansion phase have been completed. This aims to use leading technology based on bath smelting of bone-dry concentrates in a Continuous Reactor. This paper provides an overview of the relatively short plant history, its development and improvements together with operating indices achieved.

Jan 1, 1998

By Marco Olper

After two years of extensive research a new and innovative modification to the CX-EW process has been exploited. This process, called CX-EWS, avoids completely all the critical aspects of the previous process which affected the cost of the energy, of the chemicals and of The maintenance of the insoluble anodes. All these benefits reflect a saving of about 30% of The operating costs compared to the present traditional production and allow for a total operating costs of less than 6.5 cts/lb. lead (net of raw material cost). With this new technology it is allowed for the first time the treatment in the same plant facilities of both primary lead sulphide concentrate and spent batteries. The paper describes the technical and economical aspect of the new process with a feasibility study for 150,000 t/y spent battery facility throughput.

Jan 1, 1995

By S. P. Rivers

The stainless steel industry re1ies on nitric-hydrofluoric acid (HNO,/HF) pickling solutions to remove surface contaminants and maintain the corrosion resistance of the steel. More stringent environmental guide1ines are expected to be placed on the disposal of these solutions which could significantly increase processing costs. The U.S. Bureau of Mines has been conducting research to develop a process for recycling depleted pickling solutions, thus reducing the quantity of by product acids generated. Research has shown that F- can be liberated from the predominant iron fluoride species (FeF,') by using oxalic acid in an electrodialysis cell. Ion selective membranes allow dissolved metals in the depleted solution to be replaced with hydronium ions by metathesis, thereby regenerating the HF. The regenerated HN03/HF is then retained in the pick1ing solution. This paper reports on the research effort at the U.S. Bureau of Mines Rolla Research Center to apply electrodialytic recycling to HN03/HF pickling solutions.

Jan 1, 1993

By S. Suzuki, Y. Maeda, N. Wakamatsu

"A new pyrometallugical technology, named KLS process, has been developed by Dowa Mining at its Kosaka Smelter to smelt various kinds of lead raw materials.The process consists of clearly separated two reaction steps, smelting and reduction. For this purpose, respective stationary furnaces are installed which are connected by a slag launder.Dry raw materials, together with pulverized coal and oxygen-enriched air, are injected through a lance pipe into the molten slag in the first furnace. It is kept under a high oxygen potential to remove sulfur completely. Resultant PbO rich slag overflows to the second furnace where pulverized coal and insufficient air are also injected through a lance pipe to reduce PbO to lead bullion and to compensate for thermal deficit. The entire operation is carried out continuously. The process development started back in 1981. In late 1986, a pilot plant with a capacity of 3.5t/H was constructed.Already nearly 20,000 tons of raw materials, mostly lead sulfate mixtures have been smelted successfully.IntroductionFor a long time, main raw materials for lead smelting at Kosaka smelter have been such secondary incombustibles as lead sulfate and lead-barium sulfate. The former is leach residue of the copper smelter flue dust and the latter originates from Iijima zinc refinery. While the most of lead concentrates produced locally has been smelted by an ISF of Hachinohe smelter in which Dowa Mining has a share.The surplus lead concentrates were processed at Kosaka by a hydrometallurgical method to convert PbS to PbSO 4 as pretreatment, and followed by simultaneous smelting together with the above secondary materials (1). Approximate output has been 1,5000 /M of lead bullion and slightly more than 2,000t/M of refined lead by adding lead bullion returned back from Hachinohe smelter (2)."

Jan 1, 1988

By Yoshifumi Abe, Akinori Toraiwa

"Nippon Mining & Metals started a new copper anode slime treatment plant that processes slimes in a chloride media. The basic plan of the process was proposed by Mr. James E. Hoffmann and Nippon Mining & Metals modified and advanced to produce precious metals in acceptable qualities for the company. The process has a wet chlorination stage of decopperized slimes, a solvent extraction and a reduction stages of gold, a silver chloride reduction stage and separative reduction stage of its gold extraction raffinate. The new plant of this process started in 1997 and has been operated in good condition.IntroductionThe old anode slime treatment plant of Nippon Mining & Metals, located in it's Hitachi Refinery, processed anode slimes through a combination of pyrometarllurgical processing and electrorefining. There was a need to plan a future of the plant because the maintenance cost increased year by year and a new selenium registration was going to be applied to the plant. Some plans were discussed and the result was that the process proposed by Mr. Hoffmann was superior among them.Nippon Mining & Metals started 'to examine the process and the experimental result showed that the process had an ability to be its new process but further research should be necessary to produce precious metals in acceptable qualities. The final process flow has some modified and additional stages to be suitable for its requirement. Silver processing stage is quite changed. Gold extraction stage has a new step to polish gold loading DBC. Gold extraction raffinate treatment stage is advanced to be able to recover precious metals, selenium and tellurium, separately. Aeration under atmospheric pressure is employed in decopperizing stage.The basic design of the new plant started in 1995 and finished in 1997. The construction of the new plant began in April 1997 and finished in October. The plant has been operating well after the four months test operation."

Jan 1, 2000

By Vadym Drozd, Yongzhou Sun, Shah Najiba, Jiuhua Chen, Andriy Durygin

"Phase transitions of the potential hydrogen storage compound, ammonia borane (NH3.BH3), was investigated using Raman spectroscopy and a diamond anvil cell at high pressures up to 9.5 GPa and low temperatures down to 90K. At room temperature, ammonia borane has three phase transitions in this pressure range. Upon cooling, four new phases were discovered through changes in characteristic Raman spectra. This result provides information about the stability of new bonding characteristics of this potential hydrogen storage material at low temperature and high pressure region.IntroductionDevelopment of hydrogen technology requires the safe, efficient and environmental friendly materials for hydrogen storage and hydrides have attracted much attention as hydrogen storage media. Among chemical hydrides, ammonia borane (BH3NH3) stands out due to its high gravimetric and volumetric hydrogen density ' "". Despite high hydrogen content, this compound is very stable. It releases hydrogen in several steps by thermal decomposition in the temperature range of 100°C to 500°C. Direct thermal decomposition also causes toxic borazine emission. Recent research interests on ammonia borane include destabilizing this compound to lower the dehydrogenation temperature with an enhanced hydrogen release rate using different techniques, e.g. the nanoscaffolds'', ionic liquids"" and acid'"" or transition metal catalysts' ""'. As a molecule of ammonia borane consists of protonic (NH) and hydritic (BH) hydrogens bonded by the polarized dative bond, thermal or catalyzed decomposition requires breaking of N-H and B-H bonding. Still now, the detailed information about the bonding characteristics of ammonia borane is not sufficient to understand details about its phases and structures. The development of methods to enhance hydrogen discharge rate from ammonia borane requires a detailed study about the structural and dynamical properties that control the stability and the intermolecular interactions of this material. This study is motivated to investigate the stability of the existing phases and also to explore the existence of any new phases at different temperatures and pressures which may have enhanced hydrogen release and uptake properties."

Jan 1, 2012

By K. J. Richards

The converting of copper mattes to blister copper has seen few technical advances since the introduction of batch furnaces using submerged tuyeres over a hundred years ago. The first side-blown converting vessel, operated by P. Manhes in 1882, was an offshoot of the 'Bessemer steelmaking process, and subsequent improvements in the conversion of molten mattes resulted In the Peirce-Smith converter, still the Industry standard today. While Peirce-Smith' converting has served the industry well since the early 1900!s, increasingly stringent environmental regulations, burgeoning energy costs, and a trend toward continuous processing have set the stage for a major improvement in this area of copper production. In contrast to a growing number of approaches for continuous converting using molten copper mattes, Kennecott is developing a process for treatment of solidified matte which allows improved' control, higher oxygen enrichment and a separation or decoupling of smelting and converting operations not possible with the other converting technologies. The new process known as Solid Matte Oxygen Converting, or SMOC, eliminates the need for molten matte transfers, minimizes fugitive emissions, and produces high strength SO2 off gases which substantially reduce offgas handling requirements. The SMOC process, despite additional matte solidification and size reduction steps, offers both capital and operating cost advantages for new smelters and the upgrading of existing plants, when compared with conventional converting technologies. Capital cost reductions of up to 35% in converting, gas handling, and sulfur fixation are indicated. Kennecott has successfully tested the new process concept and continued' development work is now under way to commercialize the technology. This paper reviews the limitations of batch copper converting with emphasis on the need for a continuous process, previous industry approaches to continuous converting of molten mattes, and the new Kennecott development.

Jan 1, 1983

By Michel Boisvert

Noranda Metallurgy is presently completing construction of the new Noranda Converter (NCV) at its Home Smelter in Rouyn-Noranda. This capital investment of CDN$56M is the continuation of the Emissions and SO2 Reduction Program that was initiated in the late 1980s with the acid plant for Reactor off-gas treatment. The Patented Noranda Converter was developed and pilot tested at the Home Smelter in the early 1990s. The project will replace the Peirce-Smith Converters and enable sulphur fixation to be 'increased from 70% to over 90% by 2002 with an accompanying reduction of dust emissions to the atmosphere. The construction site is an extension of the present Noranda Reactor area. A number of existing facilities including the acid plant and process air supply were used to minimize the capital cost of the project. This paper provides a brief history of the Noranda converting process, the Home Smelter Emissions and SO2 Reduction Program, ,project implementation and construction, a description of the different facilities, and preparation of human resources for start-up.

Jan 1, 1998

By llya Perederiy, Vladimiros G. Papangelakis, Indje Mihaylov

"Nickel slags obtained from various smelting furnaces and converters differ in terms of their chemical composition and microstructure. The microstructure of the slag is largely affected by how fast the slag is cooled after being discharged from the furnace. Slow cooling is known to promote crystallization and growth of phases such as crystalline fayalite (Fe2Si04), magnetite (Fe3Ü4) and vitreous silica (S1O2). Slag granulation causes rapid solidification of the melt in the form of either an amorphous solid or highly intergrown crystalline silicate and oxide phases. Smelter slags contain entrapped Ni, Co and Cu in the form of dissolved oxides and matte inclusions. Extraction of the entrapped metals by high pressure oxidative acid leaching (250°C, 70 g/L initial H2SO4, up to 90 psi O2, 45 min) relies on the dissolution of the metal bearing minerals. The impact of the slag microstructure on the accessibility of these minerals to leaching, as well as the morphology of the produced residues is discussed in this paper.IntroductionIt was shown previously that entrapped base metals can be efficiently extracted from naturally cooled (as opposed to granulated) crystalline nickel smelter and converter slags using high pressure oxidative acid leaching operating at 250°C, ~40 g/L terminal acid and 60 to 90 psig oxygen overpressure [1, 2,3,4, 5, 6].Mineral characterization work performed on a naturally cooled crystalline nickel furnace slag from Vale's operations in Sudbury (ON, Canada) was previously reported [4]. Fayalite (Fe2Si04) and magnetite (Fe3U4) were detected using powder X-ray diffraction. These two minerals as well as silica (S1O2) and matte ([Fe,Ni,Cu]Sx) were also identified with the help of energy dispersive X-ray spectroscopy (EDX) on cross-sectional images obtained with a scanning electron microscope (SEM) operating in the backscattered mode. Nickel converter slags obtained from Vale's operations in Sudbury were found to be mineralogically similar to the furnace slag, but with higher contents of matte entrainment and magnetite based on the SEM-EDX observations [6]."

Jan 1, 2012

By D. Lui, B. G. Thomas, B. Ho

"Results from mathematical models and plant experiments are combined to quantify the effect of transverse depressions and oscillation marks on heat transfer in the continuous casting mold. A heat transfer model has been developed to calculate transient heat conduction within the solidifying steel, coupled with the steady-state heat conduction with the continuous casting mold wall. The model features a detailed treatment of the interfacial gap between the shell and mold, including mass and momentum balances on the solid and liquid powder layers. The model predicts the solidified shell thickness down the mold, temperature in the mold and shell, thickness of the resolidified and liquid powder layers, heat flux distribution down the mold, mold water temperature rise, ideal taper of the mold walls, and other related phenomena. The important effect of non-uniform distribution of superheat is incorporated using the results from previous 3-D turbulent fluid flow calculations within the liquid cavity. Results from plant experiments confirm that transverse surface depressions and oscillation marks form at the meniscus and move down the mold. Measurements of mold thermocouple temperatures and breakout shell thickness were used to calibrate the models. The results indicate that the surface depressions and oscillation marks are filled with mold flux, but still have a significant effect on decreasing heat transfer. The predicted mold temperature fluctuations are consistent with measurements. If the depressions become filled with air, their effect is greatly increased. These results should be useful in the difficult task of interpreting transient mold thermocouple signals for on-line quality monitoring.IntroductionMany different types of intermittent surface defects on steel slabs arise during initial solidification in the mold of the. continuous casting machine. These defects include deep oscillation marks, surface depressions, and cracks. They may lead to quality problems, such as slivers, in the final rolled product. In severe cases, breakouts may occur, where liquid steel bursts through a thin section of the shell and drains over the casting machine below the mold."

Jan 1, 1997

By R. E. Johnson

The No. 3 reverberatory furnace at Phelps Dodge. Corporation's Morenci, Arizona copper smelter first received oxygen from a new oxygen plant during October 1982 and began operation with oxygen-fuel and oxygen sprinkle smelting burners which burn concentrate with oxygen. The furnace was completely converted to roof-mounted oxygen-fuel firing in October 1982. All conventional air-fuel bridge wall burners were extinguished at that time. The novel arch-mounted oxygen sprinkle smelting system began continuous operation April 1983. Since startup, unit fuel requirements decreased and furnace throughput significantly increased. Furnace off gas SO2 strength increased from an average of 1.5% SO2 to an average of 20% using only oxy-fuel burners. Oxygen sprinkle burner operation also has given excellent results, with the furnace off gas strength increasing to 35%-60% S02. There has been a reduction in overall arch temperatures, an increase in matte and slag temperatures, and a lowering of furnace bottom buildup with oxygen smelting. Furnace off gas is blended with converter off gas and treated in a sulfuric acid plant.

Jan 1, 1983

By Doon Gibbs

In this talk, we review highlights of x-ray magnetic scattering studies performed during the last decade, concentrating at the beginning on experiments on the rare earth metal holmium.(1-4) Besides intrinsic interest in the x-ray scattering cross-section and its description, studies of this type are motivated by the possibility that new structural and magnetic properties of rare earth metals might be revealed, and that new techniques may thereby be developed. As a result, interest in x-ray magnetic scattering experiments. has grown rapidly during the last 10 years particularly, with the regular application of synchrotron radiation techniques- Magnetic scattering experiments have by now been performed at most of the x-ray synchrotrons around the world. In addition, insertion .device beamlines dedicated to x-ray magnetic scattering experiments are planned at each of the next-generation storage rings presently under construction in the United States (APS), Europe (ESRF), and Japan (SPRING-8). Generally, the results of x-ray magnetic scattering experiments may be analyzed within two regimes of the incident x-ray energy, namely, in the limit of high x-ray energies, when the incident x-ray energy lies above the excitation energy of any absorption edge, and at resonance, when the incident energy lies near an absorption edge. In the high energy limit, the amplitude for x-ray magnetic scattering has the simple form [L(Q)?A + S(Q)?B](5-7) Here, L(Q) and S(Q) refer to the Fourier 'transforms of the atomic orbital and spin magnetization densities, respectively, and the vectors A and B depend on the incident and scattered wavevectors and on the: incident and scattered polarization vectors. 7) Because the vectors A and B are not identical, the polarization dependence of the orbital contribution to the magnetic cross-section differs from that of the spin contribution. This leads to the possibility that the orbital and spin magnetization densities maybe distinguished, in x-ray scattering experiments. The same distinction is not directly possible by neutron diffraction techniques (in dipole approximation, where the polarization dependence of the orbital contribution is identical to that of the spin contribution), and is important to a fundamental understanding of the electronic structure of magnetic materials. A particular

Jan 1, 1992

By Shufang Ding, Fukun Yan, Zhiqiang Shan, Wei Chen, Cuicui Ji

"To remove aluminum ion from chlorinated rare earth solution, this paper used hydrolysis method to explore the hydrolysis behavior of aluminum ion in aluminum chloride solution and confirm the optimum conditions of aluminum ion hydrolysis, which are pH value, temperature and initial concentration of Al203 and so on. The experimental results show that single treatment can make aluminum precipitation rates of chlorinated rare earth solution reach about 90% by hydrolysis precipitation; and then several recycle disposal can get precipitation rates of 89% for aluminum and 2.86% for rare earth.IntroductionIn China, rare earth resources are very rich and unique minerals, complete variety, and rare earth products are very large in the domestic reserves. Rare-earth and application products have been deep into all areas of our life, permanent magnet material of rare earth is one of the most popular application areas[11. Binary oxides such as praseodymium neodymium have been widely applied in the fields of glass, ceramics, magnetic materials, catalysts and so on. Especially, the advent of the Pr-Nd-Fe-B magnets which makes the world magnetic material into a new stage of development [2•3]With the development of science and technology, for industrial, physical and chemical indicators of raw materials Pr-Nd oxides (such as particle size, specific surface area and non rare earth impurities etc.) are also getting higher and higher. The oxide size has an important influence on sludge formation in the electrolytic process. If the size is too large, added oxides have settled on the bottom of slot before melting, and then generated sludge; if the particle is too small, it can cause dust dispersion, enlarge oxide unit consumption and increase the cost of production in the charging process. Some early processes use oxalic acid to make chloride neodymium praseodymium settle, and impurity can be removed cleanly, but the cost is high, it is not suitable for production. At present, most enterprises are using ammonium hydrogen carbonate to precipitate chlorinated neodymium praseodymium, but chlorinated neodymium praseodymium such as iron and aluminum and so on can easily form gel in the precipitation process, seriously affect the growth of neodymium praseodymium carbonate crystal and often leads to particle meticulous, even may also generate gel-like neodymium praseodymium sediments and cause centrifugal or suction filtration difficult. Now the actions and their removal of impurity such as iron and aluminum have done a lot of research in the production process of rare earth, removing aluminum craft with alkaline (sodium hydroxide) and acid (oxalic acid) has good effect, but the cost is higher[41; used adding complex agent to remove aluminum method which is simple and easy to operate, but aluminum removal rate is not high, and also changed the sediment of crystal type[51, and etc. This paper discusses the removal of chlorine from rare earth solution on the basis of the hydrolysis property differences betweenAJ3+ and rare earth ion."

Jan 1, 2013

By Alexey T. Kovalev, Irina A. Khabarova, Valentine A. Chanturiya, Igor Zh. Bunin, Elizaveta V. Koporulina

"The paper presents new theoretical and experimental results about mechanisms of disintegration of mineral complexes and structural transformations of the sulfide surface under high-power nanosecond electromagnetic pulses (HPEMP). The heated gas outflow from nanosecond breakdown channels of sulfide minerals under HPEMP is considered. It is shown that the gas outflow from channels can be an additional destructive factor in the processes of the electric pulse discharge disintegration of mineral complexes. It is shown that the effect of HPEMP changes chemical surface composition and, respectively, technological properties of pyrrhotite and pentlandite. Morphology and elementary composition of new micro- and nanoformations on mineral surface of pentlandite and pyrrhotite have been investigated using up-to-date methods of SEM/EDX and Scanning Probe Microscopy. Preliminary electropulse effect on mineral products before flotation allows producing optimal conditions for flotation separation of pentlandite and pyrrhotite owing to forming the new nanophases and defects on the surface of sulfides.IntroductionThe effectiveness of High-Power Nanosecond Pulses in the disintegration and liberation of fine disseminated mineral complexes and the recovery of micro- and nanoparticles of precious metals from refractory ores was demonstrated in [1, 2]. Possible mechanisms of selective disintegration were considered in [1-3]. It has been shown both theoretically and experimentally that electric breakdowns can play an important role in the nanosecond pulsed treatment of milled minerals (e.g., semiconductor sulfides and quartz with particle sizes of 100 µm to 2-3 mm) that are carriers of finely disseminated gold and other valuable components. Electric discharges in such minerals are accompanied by a destruction of integrity in the form of breakdown channels and the formation of a system of cracks around these channels [3]. The development of the domains of induced cracks around the channels is determined by the pressure of evaporated material in the breakdown channel. Upon an instantaneous energy release in a channel (nanosecond discharges), the change in its transverse size and in the gas density and pressure in the channel is determined by (i) the radial motion of the evaporation wave, (ii) the radial expansion of the channel, and (iii) the heated gas outflow from the channel. The evaporation wave moves with a speed on the same order of magnitude as the speed of sound (or greater) and travels a distance of around the initial channel radius, i.e., a much smaller distance than the breakdown channel length."

Jan 1, 2011

By Thomas M. Harris

To avoid the escalating cost of disposal of metals-containing wastewater and residues, new wastewater treatments will focus on the recovery of the metals. A combination of ion exchange and electrowinning can produce water suitable for discharge and relatively pure metals. The use of a chelating resin can enhance the selectivity of both the removal process and the elution of metals from the resin. A new, simple method of preparing a variety of chelating resins is being developed. The materials produced by this method exhibit interesting, as well as potentially useful, elution behavior. The performance of one test resin is described.

Jan 1, 1992

By Hiromichi Ohta

Precise thermal properties of molten materials are essentially required for analyzing the metal production process. These properties are also important as a clue to consider the dynamic structure of liquid materials. However, it is difficult to obtain the precise thermal diffusivity values of molten oxides at high temperature because of the experimental uncertainties arising from the bubble formation or the severe separation of radiative and conductive heat components. Recently a novel laser flash method has also developed for measuring thermal diffusivity of molten oxides at high temperature. In this new technique, the sample is melted in a metal crucible and heated to the desired temperature. A single laser pulse is flashed on the bottom of the metal crucible and the infrared ray irradiated from the same bottom surface is measured for obtaining the temperature decay, from which the thermal diffusivity of the liquid sample can be estimated. The usefulness and validity of this new laser flash technique have been confirmed by obtaining the thermal diffusivity values of silicate melts in the wide temperature range between 773 and 1673 K.

Jan 1, 2003

By Suzanne Young

The effect of LiF additions on liqt.1id1.:1s temperature and electrical conductivity over a wide range of cryolite bath ratios (1.0 to 1.5 weight ratio) was investigated. Results did not agree with multi-regression equations reported by Dewing and Choudhary over the entire region. New regression equations were developed. Reasons? are given for the differences. The models are used to discuss the economic implications of LiF additions to Hali cell electrolytes.

Jan 1, 1985

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