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In Situ Electron Microscopy of Helium Bubble Implantation in Metal Hydrides

Hattar, Khalid M.; Bufford, Daniel C.; Robinson, David; Snow, Clark S.

Here we investigated the microstructural response of various Pd physically vapor deposited films and Er and ErD2 samples prepared from neutron Tube targets to implanted He via in situ ion irradiation transmission electron microscopy and subsequent in situ annealing experiments. Small bubbles formed in both systems during implantation, but did not grow with increasing fluence or a short duration room temperature aging (weeks). Annealing produced large cavities with different densities in the two systems. The ErD2 showed increased cavity nucleation compared to Er. The spherical bubbles formed from high fluence implantation and rapid annealing in both Er and ErD2 cases differed from microstructures of naturally aged tritiated samples. Further work is still underway to determine the transition in bubble shape in the Er samples, as well as the mechanism for evolution in Pd films.

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TYPE Other Report YEAR 2014
DOIOSTI

Anisotropic radiation-induced segregation in 316L austenitic stainless steel with grain boundary character

Acta Materialia

Barr, Christopher M.; Vetterick, Gregory A.; Unocic, Kinga A.; Hattar, Khalid M.; Bai, Xian M.; Taheri, Mitra L.

Radiation-induced segregation (RIS) and subsequent depletion of chromium along grain boundaries has been shown to be an important factor in irradiation-assisted stress corrosion cracking in austenitic face-centered cubic (fcc)-based alloys used for nuclear energy systems. A full understanding of RIS requires examination of the effect of the grain boundary character on the segregation process. Understanding how specific grain boundary structures respond under irradiation would assist in developing or designing alloys that are more efficient at removing point defects, or reducing the overall rate of deleterious Cr segregation. This study shows that solute segregation is dependent not only on grain boundary misorientation, but also on the grain boundary plane, as highlighted by markedly different segregation behavior for the Σ3 incoherent and coherent grain boundaries. The link between RIS and atomistic modeling is also explored through molecular dynamic simulations of the interaction of vacancies at different grain boundary structures through defect energetics in a simple model system. A key insight from the coupled experimental RIS measurements and corresponding defect-grain boundary modeling is that grain boundary-vacancy formation energy may have a critical threshold value related to the major alloying elements' solute segregation. © 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

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TYPE Journal Article YEAR 2014
ScopusOSTI

Synthesis and characterization of solvothermal processed calcium tungstate nanomaterials from alkoxide precursors

Chemistry of Materials

Boyle, Timothy; Yang, Pin; Hattar, Khalid M.; Hernandez-Sanchez, Bernadette A.; Neville, Michael L.; Pratt, Sarah H.

An evaluation of calcium tungsten oxide (CaWO4) nanoparticles' properties was conducted using the powders generated from an all-alkoxide solvothermal (SOLVO) route. The reaction involved a toluene/pyridine mixture of tungsten(V) ethoxide ([W(OEt)5]) with calcium bis(trimethyl silyl) amide ([Ca(N(Si(CH3)3)2]) modified in situ by a series of alcohols (H-OR) including neo-pentanol (H-OCH2C(CH 3)3 or H-ONep) or sterically varied aryl alcohols (H-OC6H3R2-2,6 where R = CH3 (H-DMP), CH(CH3)2 (H-DIP), C(CH3)3 (DBP))]. Attempts to identify the intermediates generated from this series of reactions led to the crystallographic identification of [(OEt) 4W(μ-OEt)2Ca(DBP)2] (1). Each different SOLVO generated "initial" powder was found by transmission electron microscopy (TEM) and powder X-ray diffraction (PXRD) to be nanomaterials roughly assigned as the scheelite phase (PDF 00-041-1431); however, these initial powders displayed no luminescent behavior as determined by photoluminescence (PL) measurements. Thermal processing of these powders at 450, 650, and 750 C yielded progressively larger and more crystalline scheelite nanoparticles. Both PL and cathodoluminescent (CL) emission (422-425 and 429 nm, respectively) were observed for the nanomaterials processed at 750 C. Ion beam induced luminescence (IBIL, 478 nm) appeared to be in agreement with these PL and CL measurements. Further processing of the materials at 1000 C, led to a coalescence of the particles and significant improvement in the observed PL (445 nm) and CL measurements; however, the IBIL spectrum of this material was significantly altered upon exposure. These data suggest that the smaller nanoparticles were more stable to radiation effects possibly due to the lack of energy deposits based on the short track length; whereas the larger particles appear to suffer from radiation induced structural defects. © 2013 American Chemical Society.

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TYPE Journal Article YEAR 2014
DOIOSTIScopus

Understanding and controlling low-temperature aging of nanocrystalline materials

Battaile, Corbett C.; Boyce, Brad L.; Foiles, Stephen M.; Hattar, Khalid M.; Padilla, Henry A.; Sharon, John A.

Nanocrystalline copper lms were created by both repetitive high-energy pulsed power, to produce material without internal nanotwins; and pulsed laser deposition, to produce nan- otwins. Samples of these lms were indented at ambient (298K) and cryogenic temperatures by immersion in liquid nitrogen (77K) and helium (4K). The indented samples were sectioned through the indented regions and imaged in a scanning electron microscope. Extensive grain growth was observed in the lms that contained nanotwins and were indented cryogenically. The lms that either lacked twins, or were indented under ambient conditions, were found to exhibit no substantial grain growth by visual inspection. Precession transmission elec- tron microscopy was used to con rm these ndings quantitatively, and show that 3 and 7 boundaries proliferate during grain growth, implying that these interface types play a key role in governing the extensive grain growth observed here. Molecular dynamics sim- ulations of the motion of individual grain boundaries demonstrate that speci c classes of boundaries - notably 3 and 7 - exhibit anti- or a-thermal migration, meaning that their mobilities either increase or do not change signi cantly with decreasing temperature. An in-situ cryogenic indentation capability was developed and implemented in a transmission electron microscope. Preliminary results do not show extensive cryogenic grain growth in indented copper lms. This discrepancy could arise from the signi cant di erences in con g- uration and loading of the specimen between the two approaches, and further research and development of this capability is needed.

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TYPE SAND Report YEAR 2013
DOIOSTI

In-situ transmission electron microscopy of liposomes in an aqueous environment

Langmuir

Pratt, Sarah H.; Sasaki, Darryl Y.; Kinghorn, Aubrianna N.; Hattar, Khalid M.

The characterization of liposomes was undertaken using in-situ microfluidic transmission electron microscopy. Liposomes were imaged without contrast enhancement staining or cryogenic treatment, allowing for the observation of functional liposomes in an aqueous environment. The stability and quality of the liposome structures observed were found to be highly dependent on the surface and liposome chemistries within the liquid cell. The successful imaging of liposomes suggests the potential for the extension of in-situ microfluidic TEM to a wide variety of other biological and soft matter systems and processes. © 2013 American Chemical Society.

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TYPE Journal Article YEAR 2013
DOIOSTIScopus
Results 451–500 of 613
Results 451–500 of 613