Abstract: Focused ion beam (FIB) induced damage in nanocrystalline Al thin films has been characterized using advanced transmission electron microscopy techniques. Electron tomography was used to analyze the three-dimensional distribution of point defect clusters induced by FIB milling, as well as their interaction with preexisting dislocations generated by internal stresses in the Al films. The atomic structure of interstitial Frank loops induced by irradiation, as well as the core structure of Frank dislocations, has been resolved with aberration-corrected high-resolution annular dark-field scanning TEM. The combination of both techniques constitutes a powerful tool for the study of the intrinsic structural properties of point defect clusters as well as the interaction of these defects with preexisting or deformation dislocations in irradiated bulk or nanostructured materials.

Abstract: In this work we describe the formulation and characterization of chemically modified polymeric nanocapsules incorporating the anticancer drug, quercetin, for the passive and active targeting to tumors. Folic acid was conjugated to poly(lactide-co-glycolide) (PLGA) polymer to facilitate active targeting to cancer cells. Two different methods for the conjugation of PLGA to folic acid were employed utilizing polyethylene glycol (PEG) as a spacer. Characterization of the conjugates was performed using FTIR and H-1 NMR studies. The PEG and folk acid content was independent of the conjugation methodology employed. PEGylation has shown to reduce the size of the nanocapsule; moreover, zeta-potential was shown to be polymer-type dependent. Comparative studies on the cytotoxicity and cellular uptake of the different formulations by He La cells, in the presence and absence of excess folic acid, were carried out using MTT assay and Confocal Laser Scanning Microscopy, respectively. Both results confirmed the selective uptake and cytotoxicity of the folic acid targeted nanocapsules to the folate enriched cancer cells in a folate-dependent manner. Finally, the passive tumor accumulation and the active targeting of the nanocapsules to folate-expressing cells were confirmed upon intravenous administration in He La or IGROV-1 tumor-bearing mice. The developed nanocapsules provide a system for targeted delivery of a range of hydrophobic anticancer drugs in vivo.

Abstract: A major revolution for electron microscopy in the past decade is the introduction of aberration correction, which enables one to increase both the spatial resolution and the energy resolution to the optical limit. Aberration correction has contributed significantly to the imaging at low operating voltages. This is crucial for carbon-based nanomaterials which are sensitive to electron irradiation. The research of carbon nanomaterials and nanohybrids, in particular the fundamental understanding of defects and interfaces, can now be carried out in unprecedented detail by aberration-corrected transmission electron microscopy (AC-TEM). This review discusses new possibilities and limits of AC-TEM at low voltage, including the structural imaging at atomic resolution, in three dimensions and spectroscopic investigation of chemistry and bonding. In situ TEM of carbon-based nanomaterials is discussed and illustrated through recent reports with particular emphasis on the underlying physics of interactions between electrons and carbon atoms.

Abstract: A method to correlate microstructure from cross-section transmission electron microscopy (TEM) investigations and transport properties of a single well characterized high-T-c artificial grain boundary junction is reported. A YBa2Cu3O7-delta 45 degrees twist junction exhibiting the typical phenomenology of high T-c Josephson weak links was employed. The TEM sample preparation is based on focused ion beam etching and allows to easily localize the electron transparent area on a microbridge. The reported technique opens clear perspectives in the determination of the microstructural origin of variations in Josephson junction properties, such as the spread in I-c and IcRN values and the presence of different transport regimes in nominally identical junctions. (C) 1999 American Institute of Physics. [S0003-6951(99)03404-X].

Abstract: We measured the electrical resistivity R(T) and specific heat C-p(T) between room temperature (RT) and 4.2 K as well as the microstructure by transmission electron microscopy (TEM) of a Ni-52 Ti-48 SMA quenched from 1000degreesC (B2-Phase range) to RT and then annealed for 1h at T=380degreesC, 550degreesC and 650degreesC. In the “as quenched” and the “650degreesC annealed” state no martensitic transformations (MT's) occur. The diffraction patterns show faint reflections originating from coherent Ni4Ti3 precipitates in an early state of formation. Additional reflections of the type 1/2 <110>, 1/2 <111> and 1/3 <110> result from various lattice displacement waves, which are precursors of the MT's to the B19' and R-phase, respectively. Indeed, high resolution TEM micrographs of the [001] zone of the “as quenched” sample reveal transverse 1/2 <110> <110> lattice displacement waves, precursors of the B19' martensite. The coherent Ni4Ti3 precipitates, homogeneously distributed on a small length scale, binder the MT's in the “as quenched” and the “650degreesC annealed” state, and thus only the precursors appear. When annealed at T=380degreesC, however, coherent Ni4Ti3 precipitates with a length of 10nm are clearly visible in TEM. These precipitates trigger the NIT from the B2 to the R-phase on cooling, as evidenced also by anomalies in R(T) and C-p(T). Annealing at T-550degreesC leads to the well known two step MT's from the B2 to the R-phase and then into the B19'-phase. These martensitic transitions are clearly seen as additional peaks in the specific heat and anomalies in the resistance, while the “as quenched” and 650degreesC annealed samples show weak features in R(T) and C-p(T).

Abstract: Bulk oxyfluoride glasses doped with Ag nanoclusters have been prepared using the melt quenching technique. When pumped in the absorption band of Ag nanoclusters between 300 to 500 nm, these glasses emit a very broad luminescence band covering all the visible range with a weak tail extending into the near infrared. The maximum of the luminescence band and its color shifts to the blue with a shortening of the excitation wavelength and an increasing ratio of oxide to fluoride components, resulting in white color luminescence at a particular ratio of oxide to fluoride; with a quantum yield above 20%.

Abstract: Stearate@Cu/ZnO nanocomposite particles with molar ratios of ZnO ∶ Cu = 2 and 5 are synthesized by reduction of the metalorganic Cu precursor [Cu{(OCH(CH3)CH2N(CH3)2)}2] in the presence of stearate@ZnO nanoparticles. In the case of ZnO ∶ Cu = 5, high-angle annular dark field-scanning transmission electron microscopy (HAADF-STEM) combined with electron-energy-loss-spectroscopy (EELS) as well as attenuated total reflection Fourier transform infrared (ATR-IR) spectroscopy are used to localize the small amount of Cu deposited on the surface of 35 nm sized stearate@ZnO particles. For ZnO ∶ Cu = 2, the microstructure of the nanocomposites after catalytic activity testing is characterized by HAADF-STEM techniques. This reveals the construction of large Cu nanoparticles (2050 nm) decorated by small ZnO nanoparticles (35 nm). The catalytic activity of both composites for the synthesis of methanol from syn gas is evaluated.

Abstract: Mesoporous carbon, which can be replicated from mesoporous silica and whose surface is hydrophobic, can be an ideal catalyst for the esterification of fatty acids. Here we report an easy and low cost way to prepare sulfonic acid group-functionalized mesoporous carbon. A sample of calcined mesoporous silica SBA-15 was added to an aqueous sucrose solution followed by drying and calcination at different temperatures. In contrast to existing procedures, the obtained hybrid Si/C material was then first sulfonated in H2SO4, before the final removal of the silica template in order to stabilize the porous structure towards the liquid phase sulfonation treatment. Thus the silicacarbon composites, instead of the mesoporous carbon, were successfully sulfonated to introduce SO3H groups, while keeping the ordered mesoporous structure intact. The influence of carbonization temperature was investigated, suggesting an optimum temperature of 873 K. The SO3H group-functionalized mesoporous carbon, denoted as CMK-3-873-SO3H, was characterized by means of XRD, N2 physisorption, SEM, FT-IR, elemental analysis and TEM. It followed that a uniform mesoporous carbon was obtained with an average pore size of 3.89 nm, a specific surface of 807 m2/g and a SO3H group loading of 0.39 meq/g of dry material. Compared with other solid acid catalysts, the resulting material shows enhanced activity in the acid-catalyzed esterification of oleic acid with methanol, and can be used repeatedly. The increased catalytic performance is attributed to the hydrophobic surface and larger pore size of the new catalyst. It can effectively accommodate long chain fatty acids and reject formed water, making the active sites easily accessible.