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    Studying dynamic processes of nano-sized objects in liquid using scanning transmission electron microscopy
    (Cambridge : JoVE, 2017) de Jong, Niels; Hermannsdörfer, Justus
    Samples fully embedded in liquid can be studied at a nanoscale spatial resolution with Scanning Transmission Electron Microscopy (STEM) using a microfluidic chamber assembled in the specimen holder for Transmission Electron Microscopy (TEM) and STEM. The microfluidic system consists of two silicon microchips supporting thin Silicon Nitride (SiN) membrane windows. This article describes the basic steps of sample loading and data acquisition. Most important of all is to ensure that the liquid compartment is correctly assembled, thus providing a thin liquid layer and a vacuum seal. This protocol also includes a number of tests necessary to perform during sample loading in order to ensure correct assembly. Once the sample is loaded in the electron microscope, the liquid thickness needs to be measured. Incorrect assembly may result in a too-thick liquid, while a too-thin liquid may indicate the absence of liquid, such as when a bubble is formed. Finally, the protocol explains how images are taken and how dynamic processes can be studied. A sample containing AuNPs is imaged both in pure water and in saline.
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    Cathodoluminescence and TEM investigations of structural and optical properties of AlGaN on epitaxial laterally overgrown AlN/sapphire templates
    (Milton Park : Taylor & Francis, 2013) Zeimer, U.; Mogilatenko, A.; Kueller, V.; Knauer, A.; Weyers, M.
    Surface steps as high as 15 nm on up to 10 μm thick AlN layers grown on patterned AlN/sapphire templates play a major role for the structural and optical properties of AlxGa1−xN layers with x ≥ 0.5 grown subsequently by metalorganic vapour phase epitaxy. The higher the Ga content in these layers is, the stronger is the influence of the surface morphology on their properties. For x = 0.5 not only periodic inhomogeneities in the Al content due to growth of Ga-rich facets are observed by cathodoluminescence, but these facets give rise to additional dislocation formation as discovered by annular dark-field scanning transmission electron microscopy. For AlxGa1−xN layers with x = 0.8 the difference in Al content between facets and surrounding material is much smaller. Therefore, the threading dislocation density (TDD) is only defined by the TDD in the underlying epitaxially laterally overgrown (ELO) AlN layer. This way high quality Al0.8Ga0.2N with a thickness up to 1.5 μm and a TDD ≤ 5x108 cm−2 was obtained.
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    GaN-based radial heterostructure nanowires grown by MBE and ALD
    (Bristol : Institute of Physics Publishing, 2013) Lari, L.; Ross, I.M.; Walther, T.; Black, K.; Cheze, C.; Geelhaar, L.; Riechert, H.; Chalker, P.R.
    A combination of molecular beam epitaxy (MBE) and atomic layer deposition (ALD) was adopted to fabricate GaN-based core/shell NW structures. ALD was used to deposit a HfO2 shell of onto the MBE grown GaN NWs. Electron transparent samples were prepared by focussed ion beam methods and characterized using state-of-the-art analytical transmission and scanning transmission electron microscopy. The polycrystalline coating was found to be uniform along the whole length of the NWs. Photoluminescence and Raman spectroscopy analysis confirms that the HfO2 ALD coating does not add any structural defect when deposited on the NWs.
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    Nanoscale spectroscopic imaging of GaAs-AlGaAs quantum well tube nanowires: Correlating luminescence with nanowire size and inner multishell structure
    (Berlin : De Gruyter, 2019) Prete, P.; Wolf, D.; Marzo, F.; Lovergine, N.
    The luminescence and inner structure of GaAs-AlGaAs quantum well tube (QWT) nanowires were studied using lowerature cathodoluminescence (CL) spectroscopic imaging, in combination with scanning transmission electron microscopy (STEM) tomography, allowing for the first time a robust correlation between the luminescence properties of these nanowires and their size and inner 3D structure down to the nanoscale. Besides the core luminescence and minor defects-related contributions, each nanowire showed one or more QWT peaks associated with nanowire regions of different diameters. The values of the GaAs shell thickness corresponding to each QWT peak were then determined from the nanowire diameters by employing a multishell growth model upon validation against experimental data (core diameter and GaAs and AlGaAs shell thickness) obtained from the analysis of the 3D reconstructed STEM tomogram of a GaAs-AlGaAs QWT nanowire. We found that QWT peak energies as a function of thus-estimated (3-7 nm) GaAs shell thickness are 40-120 meV below the theoretical values of exciton recombination for uniform QWTs symmetrically wrapped around a central core. However, the analysis of the 3D tomogram further evidenced azimuthal asymmetries as well as (azimuthal and axial) random fluctuations of the GaAs shell thickness, suggesting that the red-shift of QWT emissions is prominently due to carrier localization. The CL mapping of QWT emission intensities along the nanowire axis allowed to directly image the nanoscale localization of the emission, supporting the above picture. Our findings contribute to a deeper understanding of the luminescence-structure relationship in QWT nanowires and will foster their applications as efficient nanolaser sources for future monolithic integration onto silicon.