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Studying localized corrosion using liquid cell transmission electron microscopy

Chemical Communications

Chee, See W.; Pratt, Sarah H.; Hattar, Khalid M.; Duquette, David; Ross, Frances M.

Localized corrosion of Cu and Al thin films exposed to aqueous NaCl solutions was studied using liquid cell transmission electron microscopy (LCTEM). We demonstrate that potentiostatic control can be used to initiate pitting and that local compositional changes, due to focused ion beam implantation of Au+ ions, can modify the corrosion susceptibility of Al films. This journal is

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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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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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Application of in-situ ion irradiation TEM and 4D tomography to advanced scintillator materials

Proceedings of SPIE - The International Society for Optical Engineering

Pratt, Sarah H.; Hattar, Khalid M.; Boyle, Timothy; Villone, Janelle; Yang, Pin; Doty, F.P.; Hernandez-Sanchez, Bernadette A.

Scintillating nanomaterials are being investigated as replacements for fragile, difficult to synthesize single crystal radiation detectors, but greater insight into their structural stability when exposed to extreme environments is needed to determine long-term performance. An initial study using high-Z cadmium tungstate (CdWO4) nanorods and an in-situ ion irradiation transmission electron microscope (I3TEM) was performed to determine the feasibility of these extreme environment experiments. The I3TEM presents a unique capability that permits the real time characterization of nanostructures exposed to various types of ion irradiation. In this work, we investigated the structural evolution of CdWO4 nanorods exposed to 50 nA of 3 MeV copper (3+) ions. During the first several minutes of exposure, the nanorods underwent significant structural evolution. This appears to occur in two steps where the nanorods are first segmented into smaller sections followed by the sintering of adjacent particles into larger nanostructures. An additional study combined in-situ ion irradiation with electron tomography to record tilt series after each irradiation dose; which were then processed into 3D reconstructions to show radiation damage to the material over time. Analyses to understand the mechanisms and structure-property relationships involved are ongoing. © 2012 SPIE.

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Results 1–25 of 28
Results 1–25 of 28