Elasticity of Cross-Linked Titania Nanocrystal Assemblies Probed by AFM-Bulge Tests
In order to enable advanced technological applications of nanocrystal composites, e.g., as functional coatings and layers in flexible optics and electronics, it is necessary to understand and control their mechanical properties. The objective of this study was to show how the elasticity of such comp...
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MDPI AG
2019-08-01
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Online Access: | https://www.mdpi.com/2079-4991/9/9/1230 |
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author | Andreas Hensel Clemens J. Schröter Hendrik Schlicke Norbert Schulz Svenja Riekeberg Hoc Khiem Trieu Andreas Stierle Heshmat Noei Horst Weller Tobias Vossmeyer |
author_facet | Andreas Hensel Clemens J. Schröter Hendrik Schlicke Norbert Schulz Svenja Riekeberg Hoc Khiem Trieu Andreas Stierle Heshmat Noei Horst Weller Tobias Vossmeyer |
author_sort | Andreas Hensel |
collection | DOAJ |
description | In order to enable advanced technological applications of nanocrystal composites, e.g., as functional coatings and layers in flexible optics and electronics, it is necessary to understand and control their mechanical properties. The objective of this study was to show how the elasticity of such composites depends on the nanocrystals’ dimensionality. To this end, thin films of titania nanodots (TNDs; diameter: ~3−7 nm), nanorods (TNRs; diameter: ~3.4 nm; length: ~29 nm), and nanoplates (TNPs; thickness: ~6 nm; edge length: ~34 nm) were assembled via layer-by-layer spin-coating. 1,12-dodecanedioic acid (12DAC) was added to cross-link the nanocrystals and to enable regular film deposition. The optical attenuation coefficients of the films were determined by ultraviolet/visible (UV/vis) absorbance measurements, revealing much lower values than those known for titania films prepared via chemical vapor deposition (CVD). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images showed a homogeneous coverage of the substrates on the µm-scale but a highly disordered arrangement of nanocrystals on the nm-scale. X-ray photoelectron spectroscopy (XPS) analyses confirmed the presence of the 12DAC cross-linker after film fabrication. After transferring the films onto silicon substrates featuring circular apertures (diameter: 32−111 µm), freestanding membranes (thickness: 20−42 nm) were obtained and subjected to atomic force microscopy bulge tests (AFM-bulge tests). These measurements revealed increasing elastic moduli with increasing dimensionality of the nanocrystals, i.e., 2.57 ± 0.18 GPa for the TND films, 5.22 ± 0.39 GPa for the TNR films, and 7.21 ± 1.04 GPa for the TNP films. |
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spelling | doaj.art-2282404bebb942f8a09f29db6c5ea3662022-12-22T02:03:19ZengMDPI AGNanomaterials2079-49912019-08-0199123010.3390/nano9091230nano9091230Elasticity of Cross-Linked Titania Nanocrystal Assemblies Probed by AFM-Bulge TestsAndreas Hensel0Clemens J. Schröter1Hendrik Schlicke2Norbert Schulz3Svenja Riekeberg4Hoc Khiem Trieu5Andreas Stierle6Heshmat Noei7Horst Weller8Tobias Vossmeyer9Institute of Physical Chemistry, University of Hamburg, Grindelallee 117, D-20146 Hamburg, GermanyInstitute of Physical Chemistry, University of Hamburg, Grindelallee 117, D-20146 Hamburg, GermanyInstitute of Physical Chemistry, University of Hamburg, Grindelallee 117, D-20146 Hamburg, GermanyInstitute of Microsystems Technology, Hamburg University of Technology, Eißendorfer Straße 42, D-21073 Hamburg, GermanyInstitute of Microsystems Technology, Hamburg University of Technology, Eißendorfer Straße 42, D-21073 Hamburg, GermanyInstitute of Microsystems Technology, Hamburg University of Technology, Eißendorfer Straße 42, D-21073 Hamburg, GermanyDeutsches Elektronen-Synchrotron (DESY), Notkestraße 85, D-22607 Hamburg, GermanyDeutsches Elektronen-Synchrotron (DESY), Notkestraße 85, D-22607 Hamburg, GermanyInstitute of Physical Chemistry, University of Hamburg, Grindelallee 117, D-20146 Hamburg, GermanyInstitute of Physical Chemistry, University of Hamburg, Grindelallee 117, D-20146 Hamburg, GermanyIn order to enable advanced technological applications of nanocrystal composites, e.g., as functional coatings and layers in flexible optics and electronics, it is necessary to understand and control their mechanical properties. The objective of this study was to show how the elasticity of such composites depends on the nanocrystals’ dimensionality. To this end, thin films of titania nanodots (TNDs; diameter: ~3−7 nm), nanorods (TNRs; diameter: ~3.4 nm; length: ~29 nm), and nanoplates (TNPs; thickness: ~6 nm; edge length: ~34 nm) were assembled via layer-by-layer spin-coating. 1,12-dodecanedioic acid (12DAC) was added to cross-link the nanocrystals and to enable regular film deposition. The optical attenuation coefficients of the films were determined by ultraviolet/visible (UV/vis) absorbance measurements, revealing much lower values than those known for titania films prepared via chemical vapor deposition (CVD). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images showed a homogeneous coverage of the substrates on the µm-scale but a highly disordered arrangement of nanocrystals on the nm-scale. X-ray photoelectron spectroscopy (XPS) analyses confirmed the presence of the 12DAC cross-linker after film fabrication. After transferring the films onto silicon substrates featuring circular apertures (diameter: 32−111 µm), freestanding membranes (thickness: 20−42 nm) were obtained and subjected to atomic force microscopy bulge tests (AFM-bulge tests). These measurements revealed increasing elastic moduli with increasing dimensionality of the nanocrystals, i.e., 2.57 ± 0.18 GPa for the TND films, 5.22 ± 0.39 GPa for the TNR films, and 7.21 ± 1.04 GPa for the TNP films.https://www.mdpi.com/2079-4991/9/9/1230composite filmbulge testAFMtitaniananoparticlelayer-by-layerattenuation coefficientelastic modulusYoung’s modulusXPS |
spellingShingle | Andreas Hensel Clemens J. Schröter Hendrik Schlicke Norbert Schulz Svenja Riekeberg Hoc Khiem Trieu Andreas Stierle Heshmat Noei Horst Weller Tobias Vossmeyer Elasticity of Cross-Linked Titania Nanocrystal Assemblies Probed by AFM-Bulge Tests Nanomaterials composite film bulge test AFM titania nanoparticle layer-by-layer attenuation coefficient elastic modulus Young’s modulus XPS |
title | Elasticity of Cross-Linked Titania Nanocrystal Assemblies Probed by AFM-Bulge Tests |
title_full | Elasticity of Cross-Linked Titania Nanocrystal Assemblies Probed by AFM-Bulge Tests |
title_fullStr | Elasticity of Cross-Linked Titania Nanocrystal Assemblies Probed by AFM-Bulge Tests |
title_full_unstemmed | Elasticity of Cross-Linked Titania Nanocrystal Assemblies Probed by AFM-Bulge Tests |
title_short | Elasticity of Cross-Linked Titania Nanocrystal Assemblies Probed by AFM-Bulge Tests |
title_sort | elasticity of cross linked titania nanocrystal assemblies probed by afm bulge tests |
topic | composite film bulge test AFM titania nanoparticle layer-by-layer attenuation coefficient elastic modulus Young’s modulus XPS |
url | https://www.mdpi.com/2079-4991/9/9/1230 |
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