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Application of FIB/SEM/EDXS tomographic spectral imaging and multivariate statistical analysis to the analysis of localized corrosion

2012 IEEE Statistical Signal Processing Workshop, SSP 2012

Kotula, Paul G.; Van Benthem, Mark V.; Sorensen, Neil R.

Tomographic spectral imaging is a powerful technique for the 3D analysis of materials. The present work describes the application of this technique to the analysis of localized corrosion of a connector pin. Implemented via serial sectioning in a focused ion-beam/scanning electron microscope, electron-excited x-ray spectra were acquired from each voxel in a 3D array. The resultant tomographic spectral image was analyzed in its entirety with Sandia's Automated eXpert Spectral Image Analysis multivariate statistical analysis software. The result of the analysis is a small number of chemical components which describe the 3D phase distribution in the volume of material sampled. © 2012 IEEE.

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Cubic erbium trihydride thin films

Thin Solid Films

Adams, D.P.; Rodriguez, Marko A.; Romero, Juan A.; Kotula, Paul G.; Banks, J.C.

High-purity, erbium hydride thin films have been deposited onto α-Al 2O 3 and oxidized Si by reactive sputtering methods. Rutherford backscattering spectrometry and elastic recoil detection show that films deposited at temperatures of 35, 150 and 275°C have a composition of 3H:1Er. Erbium trihydride films consist of a face-centered cubic erbium sub-lattice with a lattice parameter in the range of 5.11-5.20 Å. The formation of cubic ErH 3 is intriguing, because previous studies demonstrate a single trihydride phase with a hexagonal metal sub-lattice. The formation of a stable, cubic trihydride phase is attributed to a large, in-plane stress resulting from ion beam sputter deposition. © 2012 Elsevier B.V. All rights reserved.

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Nanoindentation and TEM Characterization of Ion Irridiated 316L Stainless Steels

Energy Technology 2012: Carbon Dioxide Management and Other Technologies

Hattar, Khalid M.; Buchheit, Thomas E.; Kotula, Paul G.; Mcginnis, Alexander; Brewer, Luke

Understanding the effects of extensive radiation damage in structural metals provides necessary insight for predicting the performance of those metals considered for application in the extreme radiation environment. Predicting mechanical performance after long term radiation exposure is of great importance to extending the life of current nuclear reactors and for developing future materials for the next generation of reactors. A combination of finite element modeling, nanoindentation, and TEM characterization were used to rapidly determine the microstructure and mechanical properties influences of ion irradiation on a standard 316L stainless steel sample. The results of this study found that ion irradiation and small scale mechanical property testing can be used to characterize extensive levels of radiation damage structure, only when significant consideration is given to ion irradiation depth, surface roughness and polishing condition, the irradiation temperature, and.many other experimental parameters. © 2012 The Minerals, Metals, & Materials Society. All rights reserved.

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Fast lithium-ion conducting thin-film electrolytes integrated directly on flexible substrates for high-power solid-state batteries

Advanced Materials

Ihlefeld, Jon I.; Clem, Paul G.; Doyle, Barney L.; Kotula, Paul G.; Fenton, Kyle R.; Apblett, Christopher A.

By utilizing an equilibrium processing strategy that enables co-firing of oxides and base metals, a means to integrate the lithium-stable fast lithium-ion conductor lanthanum lithium tantalate directly with a thin copper foil current collector appropriate for a solid-state battery is presented. This resulting thin-film electrolyte possesses a room temperature lithium-ion conductivity of 1.5 × 10 -5 S cm -1, which has the potential to increase the power of a solid-state battery over current state of the art. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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Biomolecular interactions and responses of human epithelial and macrophage cells to engineered nanomaterials

Bachand, George B.; Brozik, Susan M.; Bachand, Marlene B.; Aaron, Jesse S.; Timlin, Jerilyn A.; Achyuthan, Komandoor A.; Kotula, Paul G.

Engineered nanomaterials (ENMs) are increasingly being used in commercial products, particularly in the biomedical, cosmetic, and clothing industries. For example, pants and shirts are routinely manufactured with silver nanoparticles to render them 'wrinkle-free.' Despite the growing applications, the associated environmental health and safety (EHS) impacts are completely unknown. The significance of this problem became pervasive within the general public when Prince Charles authored an article in 2004 warning of the potential social, ethical, health, and environmental issues connected to nanotechnology. The EHS concerns, however, continued to receive relatively little consideration from federal agencies as compared with large investments in basic nanoscience R&D. The mounting literature regarding the toxicology of ENMs (e.g., the ability of inhaled nanoparticles to cross the blood-brain barrier; Kwon et al., 2008, J. Occup. Health 50, 1) has spurred a recent realization within the NNI and other federal agencies that the EHS impacts related to nanotechnology must be addressed now. In our study we proposed to address critical aspects of this problem by developing primary correlations between nanoparticle properties and their effects on cell health and toxicity. A critical challenge embodied within this problem arises from the ability to synthesize nanoparticles with a wide array of physical properties (e.g., size, shape, composition, surface chemistry, etc.), which in turn creates an immense, multidimensional problem in assessing toxicological effects. In this work we first investigated varying sizes of quantum dots (Qdots) and their ability to cross cell membranes based on their aspect ratio utilizing hyperspectral confocal fluorescence microscopy. We then studied toxicity of epithelial cell lines that were exposed to different sized gold and silver nanoparticles using advanced imaging techniques, biochemical analyses, and optical and mass spectrometry methods. Finally we evaluated a new assay to measure transglutaminase (TG) activity; a potential marker for cell toxicity.

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Fast neutron environments

Hattar, Khalid M.; Puskar, J.D.; Doyle, Barney L.; Boyce, Brad B.; Buchheit, Thomas E.; Foiles, Stephen M.; Lu, Ping L.; Clark, Blythe C.; Kotula, Paul G.; Goods, Steven H.

The goal of this LDRD project is to develop a rapid first-order experimental procedure for the testing of advanced cladding materials that may be considered for generation IV nuclear reactors. In order to investigate this, a technique was developed to expose the coupons of potential materials to high displacement damage at elevated temperatures to simulate the neutron environment expected in Generation IV reactors. This was completed through a high temperature high-energy heavy-ion implantation. The mechanical properties of the ion irradiated region were tested by either micropillar compression or nanoindentation to determine the local properties, as a function of the implantation dose and exposure temperature. In order to directly compare the microstructural evolution and property degradation from the accelerated testing and classical neutron testing, 316L, 409, and 420 stainless steels were tested. In addition, two sets of diffusion couples from 316L and HT9 stainless steels with various refractory metals. This study has shown that if the ion irradiation size scale is taken into consideration when developing and analyzing the mechanical property data, significant insight into the structural properties of the potential cladding materials can be gained in about a week.

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Tomographic spectral imaging: Data acquisition and analysis via multivariate statistical analysis

JOM

Kotula, Paul G.; Sorensen, Neil R.

Tomographic spectral imaging is a powerful technique for the three-dimensional (3-D) analysis of materials. Using a focused ion-beam/scanning electron microscope equipped with an x-ray spectrometer, 3-D microanalysis can be performed on individual regions of a sample, such as defects, with microanalytical spatial resolution of better than 300 nm typically. The focused ion-beam can serially section at comparable thicknesses to sequentially reveal new analytical surfaces within the specimen. After each slice a full 2-spatial dimension spectral image, consisting of a complete spectrum at each point in the 2-D array, is acquired with the scanning electron microscope/energy-dispersive x-ray spectrometer on the same platform. The process is repeated multiple times to result in a 3-D or tomographic spectral image. The challenge is to effectively and efficiently analyze the tomographic spectral image to extract chemical phase distributions. Therefore, automated multivariate statistical analysis methods were developed and applied to these images. Sandia's Automated eXpert Spectral Image Analysis multivariate statistical analysis software requires no a priori information to find even very weak signals hidden in the data sets. The result of the analysis is a small number of chemical components which describe the 3-D phase distribution in the volume of material sampled. These 3-D phases can then be effectively visualized with off-the-shelf 3-D rendering software. © 2011 TMS.

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Results 201–250 of 363
Results 201–250 of 363