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A Marie Skłodowska-Curie Initial Training Network Postgraduate Research on Dilute Metamorphic Nanostructures and Metamaterials in Semiconductor Photonics Nanoscale and Atom-scale Characterization of Novel Functional Nanostructures for Photonics and Photovoltaics Atif Alam Khan ESR Cádiz INNANOMAT GROUP (MATERIALS and NANOTECHNOLOGY for INNOVATION) Department of Material Science, Metallurgical Engineering and Inorganic Chemistry, IMEYMAT Faculty of Science University of Cádiz 11510 Puerto Real, Cádiz, Spain. Date: December 8, 2016 A Marie Skłodowska-Curie Initial Training Network Postgraduate Research on Dilute Metamorphic Nanostructures and Metamaterials in Semiconductor Photonics Outline I. Personal Background II. The Project III.Project Background IV.Methodology and Instrumentation V. Present Results and Analysis VI. Summary VII.Future Works A Marie Skłodowska-Curie Initial Training Network Postgraduate Research on Dilute Metamorphic Nanostructures and Metamaterials in Semiconductor Photonics Personal Background • MSc. in Micro- and Nanotechnology • Research on Microphotolumincesce of Nanostructures • BSc. in Electrical and Electronic Engineering A Marie Skłodowska-Curie Initial Training Network Postgraduate Research on Dilute Metamorphic Nanostructures and Metamaterials in Semiconductor Photonics The Project Process Flow Aims Materials for Energy (CPV): WP3 Identification of optimum design parameters for antimony (Sb) based energy saving high efficient midinfrared (MIR) III-V solar cells (SCs), light emitting diodes (LEDs) and gas sensors (GSs) using various transmission electron microscopy (TEM) techniques. Motivation • 3.6 million GWh electric usage by 2020 • High efficient SC • Cheaper III-V photonic materials Solutions • III-Sb quantum dot (QD) IBSC and LEDs • III-Sb/Si hybrid tandem structures Optimization Modelling Morphological and Compositional analyses CPV: Concentrated Photovoltaics IBSC: Intermediate Band Solar Cell Characterization Growth TEM Processing A Marie Skłodowska-Curie Initial Training Network Postgraduate Research on Dilute Metamorphic Nanostructures and Metamaterials in Semiconductor Photonics Project Background QRs: Quantum Rings Materials QD formation wetting layer dependent Low QD density GaSb QRs for SCs GaAs Differences in lattice constants and thermal expansion coefficients Functionality barrier layer dependent: AlSb TEM Structural quality and dimensions GaxIn1-xAs/III-Sb for SCs/GSs Si AlSb/GaSb InxAl1-xAsySb1-y for SCs/GSs (Al)GaSb InAs InSb submonolayer QDs for LEDS Barrier based influences QRs shapes, density and dimensions control device performace Analyses Defect type and density Compositional distribution Designing high efficient MIR photonic devices A Marie Skłodowska-Curie Initial Training Network Methodology and Instrumentation JEOL 2010F JEOL 2100 CTEM: Diffraction contrast based morphological analysis InSb QDs InxAl1-xAsySb1-y HRTEM: Cross-sectional measurements of nanostructures Double Aberration Corrected Postgraduate Research on Dilute Metamorphic Nanostructures and Metamaterials in Semiconductor Photonics HAADF-STEM: Atomic level compositional mapping EDX: Material identification EELS: Material identification at nano-scale GaxIn1-xAs GaSb QRs FEI Titan Cubed Themis CTEM: Conventional TEM HRTEM: High Resolution TEM HAADF-STEM: High Angle Annular Dark Field-Scanning TEM EDX: Energy –dispersive X-ray EELS: Electron Energy Loss Spectroscopy A Marie Skłodowska-Curie Initial Training Network Postgraduate Research on Dilute Metamorphic Nanostructures and Metamaterials in Semiconductor Photonics Present Results and Analysis: GaSb/GaAs QRs DIFFRACTION CONTRAST GaSb QR • Low QR density (0.004-0.02/nm) GaSb WL GaSb WL • Large barrier prevents vertical stacking GaAs • No structural defect/dislocation GaAs GaSb QR • QR induced strain observed 220 bright field image 002 dark field image HAADF-STEM nanocup HAADF-STEM image • Average QR diameter = 25±3 nm • Average lobe diameter = 5±2 nm • Average lobe height = ~ 3 nm QR •HAADF images show that the QRs have the shape of nanocups A Marie Skłodowska-Curie Initial Training Network Postgraduate Research on Dilute Metamorphic Nanostructures and Metamaterials in Semiconductor Photonics Present Results and Analysis: InSb/InAs QDs DIFFRACTION CONTRAST InAs (200 nm) InSb QDs layers InAs (200 nm) • The diffraction contrast images ensure the presence of 10 InSb QDs layers with good quality. InAs (100 nm) 002DF 220BF InAs (100 nm) CTEM images HAADF-STEM Intensity profiles from column 10 of the HAADF-STEM image InAs InSb HAADF-STEM image of a QD layer region InAs Group III In: Z-> 49 As: Z-> 33 •HAADF images are sensitive to the average Z number in the atomic columns. •A new methodology based in HAADF experimental images and simulations is in progress in order to quantify the Sb distribution at atomic column resolution. •This will allow analyzing the QDs characteristics, in order to be correlated to their functional properties. In In Sb As Group V Sb: Z-> 51 Simulated intensity profile at ideal case A Marie Skłodowska-Curie Initial Training Network Postgraduate Research on Dilute Metamorphic Nanostructures and Metamaterials in Semiconductor Photonics Present Results and Analysis: InSb/(Al)GaSb QDs DIFFRACTION CONTRAST QDs layers •The analysis by diffraction contrast shows that the InSb/(Al)GaSb QDs layers have good structural quality. ATOM PROBE TOMOGRAPHY 220BF 002DF CTEM images HAADF-STEM •In this case, the existence of more than one group III elements complicate the correlation intensitycomposition from HAADF images. HAADF-STEM image of a QD layer region • Atom probe tomography (APT) analysis is in progress in order to obtain 3-dimensional (3D) information on the composition distribution of the material. • First analyses failed because of the difficulties in specimen preparation by focused ion beam (FIB) of Sb containing materials. The optimization of the preparation process is in progress. Scanning Electron Microscope (SEM) image of a FIB micro-needle sample for APT A Marie Skłodowska-Curie Initial Training Network Postgraduate Research on Dilute Metamorphic Nanostructures and Metamaterials in Semiconductor Photonics Summary • GaSb/GaAs QRs: the analysis by diffraction contrast shows low QR density of 0.0040.02/nm with no vertical stacking in the SC structure, with an overall good structural quality. The QRs have “nanocup” shape with an average diameter of ~ 25 nm. These shape and dimension based information will help finding high optical quality associated design parameters from fabrication point of view. • InSb/InAs QDs: the development of a new methodology based in HAADF-STEM experimental images and simulations is in progress in order to quantify the Sb distribution at atomic column scale, what will allow the study of the QDs size and shape. • InSb/(Al)GaSb QDs: the analysis by diffraction contrast ensures a good structural quality. APT analysis are in progress in order to obtain 3D compositional information from the material, and for this the optimization of the sample preparation by FIB is being carried out. • A Marie Skłodowska-Curie Initial Training Network Postgraduate Research on Dilute Metamorphic Nanostructures and Metamaterials in Semiconductor Photonics Skills acquired • Operating JEOL 2100 microscope to do diffraction contrast. • Interpretation of diffraction contrast images • Interpretation of HAADF-STEM images with qHAADF and MATLAB software • Conventional electron transparent TEM sample preparation techniques Outputs • Poster presentation in European Microscopy Conference (EMC) in Lyon, France in August, 2016. • Poster presentation in Molecular Beam Epitaxy (MBE) conference in Montpellier, France in September, 2016. A Marie Skłodowska-Curie Initial Training Network Postgraduate Research on Dilute Metamorphic Nanostructures and Metamaterials in Semiconductor Photonics Future Works • Analysis of InSb/InAs QDs using HAADF-STEM experimental images and MATLAB simulated data to obtain Sb composition, followed by low loss EELS experimentation for comparative analysis • Analysis of InSb/(Al)GaSb QDs samples by APT to determine In composition and hence, generating complete compositional map • Analysis of InxAl1-xAsySb1-y quaternary alloy with the help of qHAADF software and MATLAB simulations • Analysis on GaxIn1-xAs/III-Sb/Si samples • Involvement in various outreach programs • Set up a robust network platfrom that should help me advancing my career as a future expert either in industry or academy. Daniel Fernández de los Reyes Cádiz 12 12