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Here we report on the material chemistry following crystallization in the presence of water vapor of chlorinated formamidinium lead-triiodide (NH2CH = NH2PbI3−xClx) perovskite films. We found in-situ exposure to water vapor reduces, or possibly eliminates, the retention of chlorine (Cl) inside NH2CH = NH2PbI3−xClx crystals. There is a strong tendency toward Cl volatility, which indicates the sensitivity of these materials for their integration into solar cells. The requisite for additional efforts focused on the mitigation of water vapor is reported. Based on the in situ results, hot casting (<100 °C) in dry conditions demonstrates improved film coverage and Cl retention with efficiencies reaching 12.07%.
A complex cerium bearing oxide, Gd2Ce2O7 was synthesized in order to simulate Pu in a fluorite derivative oxide. X-ray diffraction (XRD) data was collected using a lab diffractometer at room temperature and analyzed by Rietveld refinement method using the xnd program. The diffraction pattern obtained from the material could be indexed as a C-type cubic bixbyite crystal structure however several peaks showed peak broadening and could not be accounted for within the single-phase bixbyite model. A full pattern refinement, assuming a possible existence of short order disordered bixbyite regions within an average disordered fluorite phase gave a good fit with the experimental data, providing an estimate for correlation length of those bixbyite regions. Transmission electron microscopy confirms the existence of these correlated domains of disordered bixbyite type phase inside a defect fluorite lattice. Understanding the extent of these domains as a function of composition and the thermal history of the samples may have a profound effect on our understanding of miscibility gaps in Re2O3-CeO2 phase diagrams. These effects could be eventually exploited to design materials with increased radiation resistance, a desired feature for oxide matrices where actinides can be safely disposed.
Oxide composites are a class of materials with potential uses for nuclear, space, and coating applications. Exploiting their promise, however, requires a detailed understanding of their interfacial structure and chemistry. Using analytical microscopy, we have examined the radiation damage behavior at the interface of a model oxide bilayer, SrTiO3/MgO. The as-synthesized SrTiO3 thin film contained both (100) and (110) oriented domains. We found that after ion beam implantation the (110) domains amorphized at a lower radiation fluence than the (100) domains. Further, a persistent crystalline layer of SrTiO3 forms at the interface even as the rest of the SrTiO3 film amorphizes. We hypothesize that the enhanced amorphization susceptibility of the (110) domains is a consequence of how charged irradiation-induced defects at the interfaces interact with the charged planes of the (110) domains. These results demonstrate the complex relationship between interfacial structure and radiation damage evolution at oxide interfaces.
Observation of growth, synthesis, dynamics, and electrochemical reactions in the liquid state is an important yet largely unstudied aspect of nanotechnology. The only techniques that can potentially provide the insights necessary to advance our understanding of these mechanisms is simultaneous atomic-scale imaging and quantitative chemical analysis (through spectroscopy) under environmental conditions in the transmission electron microscope. In this study we describe the experimental and technical conditions necessary to obtain electron energy loss (EEL) spectra from a nanoparticle in colloidal suspension using aberration-corrected scanning transmission electron microscopy (STEM) combined with the environmental liquid stage. At a fluid path length below 400 nm, atomic resolution images can be obtained and simultaneous compositional analysis can be achieved. We show that EEL spectroscopy can be used to quantify the total fluid path length around the nanoparticle and demonstrate that characteristic core-loss signals from the suspended nanoparticles can be resolved and analyzed to provide information on the local interfacial chemistry with the surrounding environment. The combined approach using aberration-corrected STEM and EEL spectra with the in situ fluid stage demonstrates a plenary platform for detailed investigations of solution-based catalysis.
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