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By Susanne Pignolet-Brandom

QEM*SEM is an automated scanning electron microscope/computer system that characterizes samples with regard to mineral modal abundances, mineral grain and particle sizes, mineral associations, and particle surface areas. Additional information, based on the classification of particles according to the area percentage of a mineral of interest, can be obtained for samples of particulates. QEM*SEM is capable of analyzing a wide variety of materials although it was originally developed for applications to the minerals industry.

Jan 1, 1988

By Graham Cooke, Abhishek Lahiri, Animesh Jha, E. Jeya Kumari

"CO2 reduction by alternative energy devices such as wind-power, electric vehicles utilize rare-earth elements (REE) in several forms; such as in piezo-electric devices, batteries and magnetic materials. In 2010, the 95% of Rare Earth supply is controlled by China, compared to USA being dominant supplier in the 1980s. The dependence upon a single source of lanthanides has prompted the utilization of lower grades of titaniferous mineral concentrates, which often have rich seams of REE. We propose a new methodology, which utilizes the low-grade minerals for the extraction of synthetic rutile and also significant quantities of REE. We demonstrate the alkali roasting of lower grades of mineral concentrates and subsequent leaching in an aqueous medium for preferential flocculation of REE during the extraction of synthetic rutile. Changes in mineral structure during alkali roasting and leaching determine flocculation of REE and permit their separation at the front end of unit process.The physical chemistry and crystal structure of minerals in equilibrium with alkali and aqueous medium play an important role, which we explain by demonstrating the changes in the crystal structure. The quantification of separation of RE oxide via chemical analysis suggests that it may be possible to separate rare-earth oxides between 50 and 80% of the initial concentration in the non-magnetic fractions of ilmenite, for example. The microstructural and X-ray diffraction analysis points out that the presence of alumina and roasting with potassium based alkali enhances the separation and flocculation of rare-earth elements at the front end of the process after roasting. The process allows the recovery of CO2 generated by recycling into the process for the regeneration of alkali."

Jan 1, 2011

By Lianjun Liu, Ying Li, Qianyi Zhang

"Photocatalytic reduction of CO2 by H2O for production of Cl fuels (CO and CH4) was studied using copper and iodine co-modified TiO2 (Cu-IffiO2) nanocomposites, with copper deposited on the surface and iodine doped in the lattice. The nanocomposites were prepared via a combined hydrothermal and wet impregnation process. All I-doped samples demonstrated visible light activity. Under UV-vis irradiation, co-modification of Cu and I significantly increased TiO2 photoactivity compared with bare TiO2 or those modified with only one species.IntroductionThe photoreduction of CO2 into fuels on photocatalysts such as TiO2 has been regarded as an important approach to solve both energy shortage and globe warming problems [1]. However, the wide band gap and fast recombination ofphotoinduced hole (h+) and electrons (e"") limited the application of TiO2 in CO2 photoreduction reaction. Extensive research has been conducted to improve the photocatalytic ability ofTiO2 by depositing or doping foreign ions that can enhance charge transfer and/or creates intra-band-gap states to induce visible light absorption at the subband- gap energy. Compared with mono-doping, co-doping of metal/nonmetal species has been reported to have higher photocatalytic activity for TiO2 [1-3]. Our previous studies showed that Cu deposited on TiO2 [4] or iodine doped in TiO2 [5] significantly enhanced the catalytic efficiency for CO2 photoreduction and increased the response to visible light. We hypothesize that there could be a synergetic effect if TiO2 is co-modified by both Cu and I species resulting in further improvement in CO2 reduction efficiency. In this work, we synthesized and characterized Cu-IffiO2 samples and investigated their activity toward CO2 reduction under visible and UV-vis illumination, respectively.Experimental MethodsMaterialsTitanium tetra-isopropoxide (TTIP, 98%) and isopropanol (C3HsO, 99.8%) were purchased from Acros Organic. Iodic acid (HIO3,99.8%) and Copper Chloride (CuCh, 99.9%) were purchased from Alfa Aesar. All other chemicals were analytical grade and used without further treatment."

Jan 1, 2012

By S. Rick Gilbert

In the course of producing a final metal product, smelters, refineries, and other metallurgical facilities produce wastes which often come under the ?scrutiny of Federal and state regulatory agencies. Many of these wastes contain combinations on zinc, copper, lead, cadmium, nickel or other metals. Frequently in the form of reverts, dusts, or sludges, these metal-containing wastes are often buried in a landfill or speculatively accumulated for future action. Environmental liability can be reduced in many cases by selecting,-a recycling facility which can re-process the waste for.' metal recovery. Encycle, at its hydrometallurgical facility Corpus Christi, has Successfully processed a variety of metallurgical by-products and wastes and returned those contained metals to commerce.

Jan 1, 1995

By Alessandro Blasi, Massimo Morgana, Corradino Sposato, Pietro Garzone, Giuseppe Devincenzis

A comparison among (2-ethylhexyl)-mono (2-ethylhexyl) ester Phosphonic acid (P507), Secondary-octyl phenoxy acetic acid (CA-12) and Bis(2,4,4-trimethylpentyl) phosphinic acid (Cyanex272), in heavy rare earths separation via hydrometallurgical processes has been investigated. The separation coefficients, , were obtained and the extraction selectivity has been evaluated using a mixture of heavy rare earths from Samarium to Ytterbium. The experimental results indicated that P507 and Cyanex 272 display a greater affinity for heavier rare earths while CA12 proved to be more effective for the lighter rare earth metals.

Jan 1, 2014

By Jose M. Gomez-Vega, Osamu Takai, Atsushi Hozumi, Hiroyuki Sugimura

"Ongoing research is reported aimed at improving the properties of mesoporous silica-based coatings on various substrates for optoelectronic or medical applications. Tetraethylorthosilicate (TEOS) was selected as the silica precursor, and amphiphilic triblock copolymers poly( ethylene oxide)- poly(propylene oxide)poly( ethylene oxide) as the surfactant micellar template or structure-directing agents. Cetyltrimethylammonium chloride (CTAC) was also used as a control agent. The effect of the templating agent and type of substrate (glass, Si, and Ti) on the mesoporosity, particularly on the alignment of the mesochannels, has been investigated. Three · different treatments (thermocalcination, photocalcination, and solvent extraction) have been also studied to remove the organic templates.IntroductionThe fabrication of mesoporous silicate-based materials through the utilization of a sol-gel process, where cooperative organization of organic and inorganic species takes place, provides a versatile approach to nanoscaled structures with potential applications in fields such as catalysts, optoelectronics, biomaterials, etc. Compared to conventional low molecular weight surfactants, self assembly of amphiphilic·block copolymers can result in mesostructured materials with larger pore sizes (up to 30 nm).1 Most of the synthetic strategies use silicon alkoxides as the silica precursor, although non-silicate metal alkoxides, e.g; Ti, Zr, Al, and B, have been also used to obtain different mesoporous materials, or even mixed metallic oxide systems. 2 Recently, Yang et al. 3 • 4 were able to synthesii:e a great variety of mesoporous metal oxides ID nonaqueous media using inorganic precursors (metal chlorides) and block copolymers as structure-directing agents."

Jan 1, 2000

By Xinghui Meng

The leaching behavior of platinum powder in .iodide solutions under oxygen pressure in an autoclave was investigated. Ammonium salts were added to the leaching solution at neutral pH as a key lixiviant for platinum. The effect of temperature, partial pressure of oxygen, concentration of iodide and of arttmonium salts on the dissolution rate of platinum was examined. Under experimental conditions, the leaching behavior of platinum powder exhibited a complex reaction mechanism. A precipitate was found during the leaching process and was identified to be platinum ammine iodide, Pt(NH3hI4. The dissolution rate was controlled by a series of chemical reactions, the equilibrium concentration of the platinum ammine iodide being responsible for the ultimate limit to the recovery.

Jan 1, 1996

By R. Hurman Eric

The electrode in a slag-resistance electric furnace is the central factor in the design and operation of the furnace by its role of conveying the smelting power, i.e. heat needed for the operation. The control parameters are the size and positioning in the slag bath which are defined by slag resistivity, furnace resistance, cell constant and power input sequence all of which are closely interrelated. The flow of heat generated by the electrode current determines the energy distributions and thus the furnace dimensions. Heat flow models concerning vertical, horizontal and combined two-dimensional flows are discussed. All these considerations are based on the experimentally determined slag properties such as its resistivity.

Jan 1, 1995

By Zhang Duomo

A novel homogenous precipitation method, including microwave heating, solution conductivity controlling and freeze drying, was developed for the preparation of US nanoparticles. The effects of the precipitation conditions on the structure and morphology of CdS particles were discussed individually. It was found that under the experimental conditions the particle sizes were controllable in the range of 14nm to 100nm. Blend-type CdS was obtained from nitrate or sulphate solution and the more stable wurtzite-type US was obtained from chloride solution, which was ascribed to the coordination of C1 and Cd2+ altering the supersaturation of the solution as well as the different growth units and their connecting patterns, In the precipitation process the surface of US nanoparticles were surface modified with CH3CHSCOOH. The results demonstrate that the bifunctional thiols of thioglycolic acid modified the surface through Cd-S coordination bonding and the induced counter ion AOT-SO3 as the balance charge further increased the stability and dispersity of US nanoparticles. This surface-modified US nanoparticles had been used to prepare nonlinear optics and self-assemble catalysts.

Jan 1, 2003

By Ann M. Hagni

"Ceramic matrix composites are inorganic materials that are particularly resistant to heat and abrasion. A magnesia (MgO) and aluminum nitride (AlN) based composite is formed by exposing a magnesia preform to a metallic alloy block in a nitrogen atmosphere at 950°C. The metallic alloy, which is composed primarily of aluminum, is wicked into the preform. Aluminum nitride matrix is grown between MgO particles as the wicked metallic aluminum reacts with nitrogen. Unused metallic alloy, remnant metallic alloy (carcass), and composite produced after 8 hours, 50 hours, and 225 hours of processing are characterized mineralogically. Reflected light microscopy, transmitted light microscopy, scanning electron microscopy, energy dispersive spectroscopy, and X-ray diffraction techniques reveal that in addition to anhedral to euhedral AhNi, AbSbSr, and Al crystallizing in the metallic alloy carcass, AIN and (Al,Si)N have formed as well. Nitride rings and nodules in the carcass may hinder AIN growth in the composite. Fine-grained residual AhNi and AhShSr are dispersed throughout the composite matrix. The nitride matrix is composed of AIN and (Al,Si)N. Rim replacement of MgO by spine! occurs in the composite. Aluminum nitrides in the metallic carcass cathodoluminesce deep violet-blue, unlike non-luminescent AIN in the composite matrix. This distinction in cathodoluminescence suggests a different mode of formation for composite AIN than for carcass AIN. Phase interpretations and textural characterizations deduced from the implementation of sophisticated mineralogical techniques have contributed to the understanding, and will aid in the improvement, of MgO/ AlN-based ceramic matrix compositeprocessing."

Jan 1, 1999

By F. H. Froes, O. N. Senkov, N. Srisukhumbowornchai

"Mechanical alloying (MA) and thermohydrogen processing (THP) approaches were used to synthesize amorphous or nanocrystalline powders of the titanium-aluminide-based alloys and composites. Fully dense samples with nanocrystalline and bimodal structures were produced from these powders by hot isostatic pressing. The stability of the microstructures during continuous heating at high temperatures was studied. Characterization techniques including X-ray diffraction, scanning and transmission electron microscopy, energy dispersive spectroscopy, and differential thermal analysis were used in this work.IntroductionAs performance demands increase, so do the demands for enhanced mechanical property combinations at reduced overall weight; and reduced weight can most efficiently be realized by the use of low-density metals with high specific strength, such as titanium alloys and titanium-aluminum intermetallics [l]. The TiAl-based alloys are attractive for high temperature applications, however, they exhibit poor ambient temperature ductility and fracture toughness [2-4]. Incremental improvements can be obtained using ingot metallurgy processing [1,2] but more substantial developments require ""far from equilibrium"" (FFE) synthesis [5-8] which allows development of novel constitutional and microstructural effects, leading to enhanced physical and mechanical properties. Improved ductility of titanium aluminide intermetallics can be achieved by disordering, grain refinement and deoxidation of the matrix, while good elevated temperature properties are achieved due to a dispersion of fine, thermodynamically stable, second phase particles.The approaches for producing nanocrystalline and amorphous TiAl-based alloys and composites used in this work included FFE powder metallurgy techniques such as rapid solidification, mechanical alloying and thermohydrogen processing. The rapid solidification (RS) technique allows extension of solubility limits, production of novel phases, and much more refined microstructures (down to nanostructure or even amorphous range) than is possible using the ingot metallurgy technique [9]. Mechanical alloying (MA) is a process in which heavy working of powder particles results in intimate alloying by repeated deformation, fracturing and welding. This process can produce greater departure from FFE than RS, leading to greater refinement effects; and additionally allows production of a dispersion of second phase particles [10]. Thermohydrogen processing involves hydrogen as a temporary alloying element in titanium to facilitate processes, refine microstructure, and improve final mechanical properties [11]; it was used in the present work to improve MA process. The combination of these three processes was expected to control the final microstructure even better than either process used alone."

Jan 1, 1998

By Yuanbo Zhang, Yongbin Yang, Guanghui Li, Zhengwei Yu, Yufeng Guo, Tao Jiang, Xiaohui Fan, Youming Hu

"Composite agglomeration process (CAP), as an innovative method for preparing blast furnace burden, was developed and has been put into operation in China. CAP is different from traditional agglomeration processes of iron-bearing materials involving sintering and pelletizing. Compared to the traditional agglomeration processes, CAP is characterized by several strengths such as permission of diverse iron-bearing materials in production, obvious improvement of permeability in the feed bed, decreasing the fuel consumption and remarkably increasing the productivity of sintering machine. Furthermore, the use of the composite agglomerates prepared with CAP is capable of obviating the negative effects caused by the differences in quality of sinter and pellets on the operation of blast furnaces. This paper mainly presents an overview of the principle and applications of CAP.Development Background and Principle of CAPhe traditional agglomeration processes including sintering and pelletizing have been the two predominant methods for preparing ironmaking burden from iron-bearing materials. Sintering is a way for agglomeration by heating the coarser fine ores (general granularity 0~10mm). The mechanical strength of irregular porous sinter is obtained by the solidification of molten phase at high temperature process. It has been shown that the production of high basicity sinter (R=1.8~2.2) is characterized by low energy consumption and high efficiency compared to low basicity sintering. Meantime, the finished high basicity sinter is characterized by good mechanical strength and metallurgical performance. Pelletizing is another way for agglomeration by firing wet green pellets, which are balled from the fine grained iron ores or concentrates. Based on the differences of chemical compositions, the finished pellets can be divided into acidic oxidized pellets, fluxed pellets, magnesium-bearing pellets, and so on. The acidic oxidized pellets are the dominant products of modern pelletizing."

Jan 1, 2012

By M. Neises, M. Roeb, C. Sattler, S. Stenger

"A two-step thermo-chemical cycle process has been developed and investigated. It is based on metal oxide redox pair systems, which can split carbon dioxide as well as water molecules by extracting oxygen atoms and reversibly incorporating them into their lattice. If concentrated solar radiation is used as the heat source, a promising method exists to produce synthesis gas from water and CO2. An easy way of operation is gained by the combination of a ceramic substrate as the absorber structure, which can be heated to high temperatures with concentrated solar radiation, and of a metal oxide coating which is capable to carry out the redox reactions. The performance and kinetics of a ferrite based redox material coated on ceramic substrates were investigated in a laboratory set-up. CO2 could be reduced with significant conversions. In addition, several side reactions were observed like the formation of carbon and like the Boudouard reaction.IntroductionThe search for alternative energy carriers and for processes able to reuse carbon dioxide stimulates the research for sustainable routes of alternative fuel production. In the scope of this search thermo-chemical processes combined with sources of concentrated solar energy have become more and more attractive. Ideally, the only raw materials for such processes are water (H2O) and carbon dioxide (CO2) enabling not only a process free of emissions, but also allow to reduce emissions of other processes by reusing CO2 to provide synthesis gas, which itself can be applied to produce chemical commodities or even better synthetic fuels like methanol or petrol.In contrast to the direct splitting of those raw materials, thermochemical cycles split water and CO2 in several steps and enable hydrogen (H2) and carbon monoxide (CO) generation at temperatures controllable by today’s technical equipment. One of the most interesting thermochemical cycles is a two-step process using metal oxide based redox systems. During the first step of this cycle (the regeneration step) the metal oxide is reduced setting some of its lattice oxygen free according to reaction (1). In the next step (the splitting) the reduced and activated material is oxidised by withdrawing oxygen from water and CO2 and at the same time hydrogen and CO is set free according to reactions (2a) and (2b) respectively."

Jan 1, 2011

By A. González

Arsenic is one of the main contaminants present in Chilean copper concentrates and its abatement represents a challenge for the process metallurgy, particularly under the strong environmental requirements in the global community. The possibility to form ferric arsenate directly from a gas phase by means of a heterogeneous reaction between an arsenic gas bearing and iron oxide was studied at laboratory scale. A thermodynamical analysis for the system Fe-As-O-S has been initially made, in order to obtain the stability conditions for the ferric arsenate or other FeAsyO2 type compounds. Experiments were made using an hematite sample suspended in a thermogravimetric device. AS4O6 gas generated from solid AS2O3 that was passed through the iron oxide sample and its instantaneous weight change was recorded directly. A kinetic study for the AS4O6 volatilization was made to control the gas composition. A chemical control between 300 and 600°C with an apparent activation energy of around 14 Kcal/mol As2O3 was determined. The samples after the reactions were chemically and XRD analysed. Arsenates detected corresponds to complex compounds. Results shows a dependence on temperature and oxygen content in the gas phase. The kinetics for iron arsenates formation is slow, reaching an arsenic capture of 6% after 80 minutes of reaction when an oxygen content of 50% is fed continuously at 800°C and 3,56% As in the gas. Experiences made at the same temperature but under higher oxygen content in a closed reactor, allowed arsenic capture close to 60%. For higher temperatures the capture is considerably lower.

Jan 1, 2003

By Chuanhong Li, Zuohua Lin, Zhancheng Guo

"Catalytic mechanism of CeO2 in combustion of coals was investigated in this paper. Catalytic combustion of four kinds of coals with different metamorphic grades by CeO2 was examined, suggesting that catalytic function of CeO2 increases with increase of metamorphic grade of the coals. One important reason for CeO2 promoting combustion of the coals is that pyrolysis of anthracite is advanced by CeO2, which not only raises the pyrolysis rate and pyrolysis conversion ratio, but increases contents of light components in pyrolysis gas; and both pore space and specific surface area of the pyrolysis char are enlarged by CeO2, which is another reason. In order to realize in situ catalysis for reducing catalyst consumption, it is crucial to increase catalyst particle number and enhance the bonding force between catalyst and coal. In addition, remarkable energy saving effect was observed when a nanometer calcium-based rare earth catalyst obtained by hydro-thermal synthesis was applied to catalytic combustion of coal injection into blast furnace.Introduction Coal combustion is acknowledged as one of the most important coal applications. Since addition of catalysts could reduce the ignition temperature of pulverized coal and accelerate the coal combustion, catalytic combustion is generally accepted as an effective measure to realize fast combustion of coal. Furthermore, different catalysts added may produce different effects on ignition temperature of coal. It is reported activity of catalysts with the same cation follows this order: OH->CO3 2->Cl->SO4 2-; while that of the catalysts which have the same anion follows: Cs+>Rb+>K+>Na+>Ba2+>Li+>Sr2+>Ca2+>Mg2+>Be2+ [1-4] .Due to the special physical and chemical structure, CeO2 plays an important role in the catalysis field. Many literatures point out that CeO2 not only has great catalytic effect on energy conversion, succeeded in catalyzing combustion of gaseous fuels such as CH4, CO, etc. but also can catalyze combustion of some liquid and solid fuels such as JP-10, black carbon, carbon deposit in the automobile exhausts and so on [5-9].Pyrolysis, the first step of combustion, directly influences ignition temperature and combustion rate of coals. So a great variety of catalysts were applied to catalyze pyrolysis of coals. And plenty of studies suggest that the alkali and alkaline-earth metal compounds inherent in the coals show apparent catalytic effect on coal pyrolysis. Meanwhile, addition of alkali and alkaline-earth metals into coal combustion process also indicates obvious catalysis effect, accelerating coal pyrolysis, improving pyrolysis conversion ratio, increasing contents of pyrolysis gases and changing composition of the pyrolysis gases [10-15].Although alkali and alkaline-earth metal compounds have good catalysis effect on coal combustion, their application in the catalysis field was limited because of their erosive attack to the combustion equipments. In contrast, CeO2, as a substitution of the traditional coal catalysts, presents widely potential application due to its good catalysis ability, non-corrosive and nontoxic. However, investigation on CeO2 catalyzing coal combustion is rarely reported. In this work, catalytic mechanism of CeO2 in coal combustion was studied, in an attempt to provide theoretical foundation for developing new catalysis technologies."

Jan 1, 2009

By Fathi Habashi

"Davy, Faraday, and Bunsen laid the foundation of electrometallurgy which had a· great impact on other areas of metallurgy. Electrometallurgy is presently dominated by the production of aluminum, the electrorefining of copper, and the electrowinning of zinc. It has also been successful in the electrowinning of copper from solutions obtained by leaching-solvent extraction. Electrowinning processes, however, are capital intensive. Improvement of the present technology should be intensely investigated especially when it is expected that such processes will increase greatly as a result of a shift from certain pyrometallurgical processes to pressure hydro metallurgy.INTRODUCTIONPyrometallurgy was used for thousands of years to produce copper and iron from their oxide ores!). Today it is still the only route to produce iron and steel and it is certain that it will remain so for many decades to come because pyrometallurgy is most suitable for the treatment of high grade oxide ores. Even when high grade iron ores are exhausted, it is possible to beneficiate the low-grade ores and produce pellets suitable for reduction in the blast furnace, which is a very efficient reactor, being a heat exchanger as well. Hydrometallurgy on the other hand can be traced to the time of alchemists in the Middle Ages when they were seeking to transmute base metals into gold, and thus were able to prepare many acids and bases which are the essential leaching agents."

Jan 1, 1997

By David Dreisinger

The cyanidation of copper containing gold ores results in the co-dissolution of copper along with gold. Copper dissolution results in elevated cyanide consumption that may make the treatment of the gold ore uneconomic. Copper-cyanide species in gold mill effluents may increase the environmental toxicity of the gold mill solutions. The objective of this study was to examine the use of solvent extraction to recover the copper cyanide species from gold mill effluents. Solvent extraction with Cognis (formerly Henkel) reagents LIX 79 and LIX 7950 was studied. Excellent extraction of copper and cyanide was achieved using pH control in extraction. Copper and cyanide may be stripped from the reagents using basic eluants. Various routes for copper and cyanide recovery from the strip solution were studied. Excellent results were obtained using electrowinning in both divided (Nation membrane) and undivided cells. Cyanide recovery was obtained by AVR treatment of a bleed stream from electrowinning. Full results of solvent extraction, copper and cyanide recovery are reported.

Jan 1, 1998

By W. L. Dalmijn

The processing of scrap and scrap cars starts with size reduction by a hammermill, or shredder. After the liberation the magnetic fraction is removed. The remaining non¬magnetic fraction mixed with other materials is screened and each fraction is processed separately. The increased use of plastic has a negative effect on the recovery of metals and waste production. At Huron Valley, Belleville Michigen, USA, the non-ferrous fraction from 5 million obsolete cars per year, containing 200,000 tons of non-ferrous metal, is processed. Aluminium Is recovered with a heavy medium separation process and concentrated with eddy current separators. The remaining heavy non-ferrous fraction is concentrated by a new combination of eddy current separation and image processing. After this separation process the zinc fraction is melted and refined and the copper, brass, stainless steel and other high-quality concentrates are sold to the secondary industries. The recycling of car scrap has become an important source of metals and materials for the secondary. materials processing industry.

Jan 1, 1995

By Lori Bassman, Cassandra George, Cullen McMahon, Md. Zakaria Quadir, Michael Ferry

"Complete and accurate analysis of subgrain microstructural features must include three-dimensional information. Three-dimensional electron backscatter diffraction (EBSD) data can be used to characterize these features; however their boundaries first must be determined. This cannot be accomplished simply with pixel-to-pixel misorientation thresholding because many of the boundaries are gradual transitions in crystallographic orientation. Fast Multiscale Clustering (FMC) is an established image processing technique that we have combined with quaternion representation of orientation to segment this kind of data. Segmentation algorithms often have issues handling images with both distinct and subtle boundaries. Our implementation of FMC addresses this by using a novel distance function and statistical analysis to take into account the variance in orientation of each feature. Although FMC was originally a twodimensional image processing algorithm it can be generalized to analyze threedimensional data sets. As an example, a segmentation of microbands in cold-rolled aluminum is presented.IntroductionThree-dimensional electron backscatter diffraction (3D-EBSD) is a method for mapping the local crystallographic orientations of points in a volume. The technique uses a dual beam platform consisting of a focused ion beam (FIB) and SEM with EBSD, where FIB is used for serial sectioning and EBSD for orientation mapping of 2D slices. These 2D slices may then be stacked to create a 3D volumetric data set.Typical uses of such a data set include characterizing the geometries and crystallographic orientations of surfaces between structures in 3D [1-5]. This involves identifying boundaries accurately, either in 2D slices with subsequent 3D reconstruction (as illustrated in Figure 1) or in the 3D data set. All such data sets present the challenges of i) aligning data slices to correct for instrument drift, ii) identifying relevant boundaries, and iii) implementing appropriate smoothing or interpolation algorithms. The focus of this paper is boundary identification."

Jan 1, 2011

By B. S. -J. Kang, M. A. Alvin, J. M. Tannenbaum

"A load-based micro-indentation technique has been developed for damage assessment and non-destructive spallation detection of TBCs at room temperature. This micro-indentation technology has been further extended to the development of a high temperature (HT) test methodology. Elastic modulus calibration tests performed on Hl 3 Tool Steel to 500°C and Haynes 230 at 1000°C displayed excellent agreement with reported values. Moreover, indentation creep tests of Haynes 230 at 1200°C were found to be in agreement with known creep exponents as well. Finally, a HT thermal flux indentation apparatus was assembled for conducting TBC turbine component testing under high temperature moisture-containing environments (= 50% steam with controlled gas content temperatures up to 1250°C). Description and design considerations of this test apparatus are discussed. Preliminary tests of ReneN5/MCrAlY/APS TBC coupons in steam/air environments with in-situ HT micro-indentation testing are conducted. Furthermore, the coupon is removed and examined for damage assessment at periodical intervals.IntroductionLoad and depth relationships acquired throughout the indentation process provide insight to material mechanical properties such as elastic modulus and hardness. Unloading segment analysis of these load displacement curves are utilized in the acquisition of a material's elastic properties. Yet, indentation tests are complex processes involving contact mechanics, material nonlinearity and even fracture mechanics. Thus exact analytical solutions for these processes are difficult to obtain. As a result, much of the current knowledge regarding the indentation process has been acquired through experimental methods and finite element simulations. Initial efforts by Tabor resulted in the application of spherical indentation to obtain post-yielding stress/strain relationships [1]. Soon thereafter, analytical load-depth relations for elastic indentation were developed [2], yet it was Lure who further derived the explicit relationships for both spherical and conical indenters [3]. Improving upon this, these interactions were later extended to indenters with various geometries by various researchers [ 4]. Additionally, by establishing the linearity of the initial unloading slope within the load-depth curve, a relationship between elastic indentation depth, maximum load, unloading slope and indenter geometry was established [5]. From this a theoretical method by which elastic modulus could be determined was established."

Jan 1, 2011