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The oxidation behaviour of tungsten disulphide (WS2) nanosheet powder with an average thickness of about 10 nm was studied in the temperature range of 25–700 °C. The samples were subjected to exposure in air in a short continuous mode as well as extended isothermal holding. It was observed that WS2 nanosheets were stable below 350 °C in air for short exposure times. A two-dimensional WS2/WO3 heterostructure evolved at 350 °C on short exposures to the oxidising atmosphere. Complete oxidation of WS2 nanosheets was observed at a temperature of about 450 °C in the continuous heating mode and at 350 °C under isothermal holding for an extended exposure time. During oxidation, WS2 nanosheets were initially transformed to 2D-WO3 nanosheets with an average thickness of about 10 nm. Significant distortion in the monoclinic structure of 2D-WO3 was observed. At higher temperatures, the WO3 nanosheets disintegrated initially to rod-shaped WO3 particles, which were subsequently transformed to thermodynamically stable spherical shaped WO3 nanoparticles. [ABSTRACT FROM AUTHOR]

The growth of gold nanoparticles and ZnO nanorods in atom beam co-sputtered Au-ZnO nanocomposite (NC) system by annealing at two different ambient conditions is demonstrated in this work. Annealing in a furnace at 600 °C (air environment) confirmed the formation of ZnO nanorods surrounded with Au nanoparticles. In-situ annealing inside a transmission electron microscope (TEM) led to the formation of gold nanocrystals with different polygonal shapes. TEM micrographs were obtained in real time at intermediate temperatures of 300 °C, 420 °C, and 600 °C under vacuum. The growth mechanisms of Au nanocrystals and ZnO nanorods are discussed in the framework of Au-Zn eutectic and Zn-melting temperatures in vacuum and air, respectively. Current-voltage responses of Au-ZnO NC nanorods in dark as well as under light illumination have been investigated and photoswitching in Au-ZnO NC system is reported. The photoswitching has been discussed in terms of Au-ZnO band-diagram. [ABSTRACT FROM AUTHOR]

The oxidation behaviour of tungsten disulphide (WS 2 ) nanosheet powder with an average thickness of about 10 nm was studied in the temperature range of 25-700 °C. The samples were subjected to exposure in air in a short continuous mode as well as extended isothermal holding. It was observed that WS 2 nanosheets were stable below 350 °C in air for short exposure times. A two-dimensional WS 2 /WO 3 heterostructure evolved at 350 °C on short exposures to the oxidising atmosphere. Complete oxidation of WS 2 nanosheets was observed at a temperature of about 450 °C in the continuous heating mode and at 350 °C under isothermal holding for an extended exposure time. During oxidation, WS 2 nanosheets were initially transformed to 2D-WO 3 nanosheets with an average thickness of about 10 nm. Significant distortion in the monoclinic structure of 2D-WO 3 was observed. At higher temperatures, the WO 3 nanosheets disintegrated initially to rod-shaped WO 3 particles, which were subsequently transformed to thermodynamically stable spherical shaped WO 3 nanoparticles.

Transmission electron microscopy (TEM) has been used intensively in investigating battery materials, e.g. to obtain phase maps of partially (dis)charged (lithium) iron phosphate (LFP/FP), which is one of the most promising cathode material for next generation lithium ion (Li-ion) batteries. Due to the weak interaction between Li atoms and fast electrons, mapping of the Li distribution is not straightforward. In this work, we revisited the issue of TEM measurements of Li distribution maps for LFP/FP. Different TEM techniques, including spectroscopic techniques (energy filtered (EF)TEM in the energy range from low-loss to core-loss) and a STEM diffraction technique (automated crystal orientation mapping (ACOM)), were applied to map the lithiation of the same location in the same sample. This enabled a direct comparison of the results. The maps obtained by all methods showed excellent agreement with each other. Because of the strong difference in the imaging mechanisms, it proves the reliability of both the spectroscopic and STEM diffraction phase mapping. A comprehensive comparison of all methods is given in terms of information content, dose level, acquisition time and signal quality. The latter three are crucial for the design of in-situ experiments with beam sensitive Li-ion battery materials. Furthermore, we demonstrated the power of STEM diffraction (ACOM-STEM) providing additional crystallographic information, which can be analyzed to gain a deeper understanding of the LFP/FP interface properties such as statistical information on phase boundary orientation and misorientation between domains., (Copyright © 2016 Elsevier B.V. All rights reserved.)