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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Main Authors: Andreas Hensel, Clemens J. Schröter, Hendrik Schlicke, Norbert Schulz, Svenja Riekeberg, Hoc Khiem Trieu, Andreas Stierle, Heshmat Noei, Horst Weller, Tobias Vossmeyer
Format: Article
Language:English
Published: MDPI AG 2019-08-01
Series:Nanomaterials
Subjects:
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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