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Nanomaterials
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Advanced Characterization Techniques for Nanomaterials
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Advanced Characterization Techniques for Nanomaterials

A special issue of Nanomaterials (ISSN 2079-4991). This special issue belongs to the section "Synthesis, Interfaces and Nanostructures".

Deadline for manuscript submissions: closed (20 December 2023) | Viewed by 8600

Special Issue Editor

Dr. Linda J. Johnston

E-Mail Website
Guest Editor
National Research Council Canada, Metrology Research Centre, Ottawa, ON, Canada
Interests: nanomaterial characterization; particle size measurements; cellulose nanomaterials; quantification of surface functional groups; metrology of nanomaterials

Special Issue Information

Dear Colleagues,

Adequate characterization of nanomaterials is essential to verify the identity and properties of the material, to ensure that related studies have used the same material and to facilitate the detection and characterization of the material in a complex environment. Nanomaterial characterization is also of increasing importance for assessing naomaterial safety for regulatory purposes. Characterization typically requires a range of methods that provide information on both chemical and physical properties and are often applied to pristine nanomaterials. However, advanced methods that utilize multiple detection and quantification methods on a single platform, greatly increasing the information content, and methods that are compatible with the detection and quantification of nanomaterials in the complex environments provided by biological or environmental samples are increasingly needed. Other challenges include assessment of the in situ behavior of nanomaterials in a dynamic environment. 

This Special Issue aims to provide an overview of recent developments in advanced characterization methods for nanomaterials with a focus on methods that combine multiple detection modes on a single platform, methods that are compatible with measurements in complex environments, and in operando methods. Both original research articles and reviews are welcome. Research areas may include (but are not limited to) the following: multimodal microscopy/spectroscopy methods, single particle methods, methods for measuring number-based concentrations of nanoparticles, characterization in complex matrices, in situ/in operando methods. 

I look forward to receiving your contributions.

Dr. Linda J. Johnston
Guest Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Nanomaterials is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2900 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • nanomaterial characterization
  • multimodal microscopy
  • single particle methods
  • complex matrices
  • in operando methods

Published Papers (8 papers)

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Research

12 pages, 7256 KiB  
Article
Spatiotemporal Visualization of Photogenerated Carriers on an Avalanche Photodiode Surface Using Ultrafast Scanning Electron Microscopy
by Yuan Tian, Dong Yang, Yu Ma, Zhongwen Li, Jun Li, Zhen Deng, Huanfang Tian, Huaixin Yang, Shuaishuai Sun and Jianqi Li
Nanomaterials 2024, 14(3), 310; https://doi.org/10.3390/nano14030310 - 3 Feb 2024
Viewed by 1128
Abstract
The spatiotemporal evolution of photogenerated charge carriers on surfaces and at interfaces of photoactive materials is an important issue for understanding fundamental physical processes in optoelectronic devices and advanced materials. Conventional optical probe-based microscopes that provide indirect information about the dynamic behavior of [...] Read more.
The spatiotemporal evolution of photogenerated charge carriers on surfaces and at interfaces of photoactive materials is an important issue for understanding fundamental physical processes in optoelectronic devices and advanced materials. Conventional optical probe-based microscopes that provide indirect information about the dynamic behavior of photogenerated carriers are inherently limited by their poor spatial resolution and large penetration depth. Herein, we develop an ultrafast scanning electron microscope (USEM) with a planar emitter. The photoelectrons per pulse in this USEM can be two orders of magnitude higher than that of a tip emitter, allowing the capture of high-resolution spatiotemporal images. We used the contrast change of the USEM to examine the dynamic nature of surface carriers in an InGaAs/InP avalanche photodiode (APD) after femtosecond laser excitation. It was observed that the photogenerated carriers showed notable longitudinal drift, lateral diffusion, and carrier recombination associated with the presence of photovoltaic potential at the surface. This work demonstrates an in situ multiphysics USEM platform with the capability to stroboscopically record carrier dynamics in space and time. Full article
(This article belongs to the Special Issue Advanced Characterization Techniques for Nanomaterials)
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20 pages, 7883 KiB  
Article
Damage Behavior with Atomic Force Microscopy on Anti-Bacterial Nanostructure Arrays
by Jonathan Wood, Richard Bright, Dennis Palms, Dan Barker and Krasimir Vasilev
Nanomaterials 2024, 14(3), 253; https://doi.org/10.3390/nano14030253 - 24 Jan 2024
Viewed by 751
Abstract
The atomic force microscope is a versatile tool for assessing the topography, friction, and roughness of a broad spectrum of surfaces, encompassing anti-bacterial nanostructure arrays. Measuring and comparing all these values with one instrument allows clear comparisons of many nanomechanical reactions and anomalies. [...] Read more.
The atomic force microscope is a versatile tool for assessing the topography, friction, and roughness of a broad spectrum of surfaces, encompassing anti-bacterial nanostructure arrays. Measuring and comparing all these values with one instrument allows clear comparisons of many nanomechanical reactions and anomalies. Increasing nano-Newton-level forces through the cantilever tip allows for the testing and measuring of failure points, damage behavior, and functionality under unfavorable conditions. Subjecting a grade 5 titanium alloy to hydrothermally etched nanostructures while applying elevated cantilever tip forces resulted in the observation of irreversible damage through atomic force microscopy. Despite the damage, a rough and non-uniform morphology remained that may still allow it to perform in its intended application as an anti-bacterial implant surface. Utilizing an atomic force microscope enables the evaluation of these surfaces before their biomedical application. Full article
(This article belongs to the Special Issue Advanced Characterization Techniques for Nanomaterials)
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16 pages, 5064 KiB  
Article
Characterization and Cellular Toxicity Studies of Commercial Manganese Oxide Nanoparticles
by Linda J. Johnston, Xiaomei Du, Andre Zborowski and David C. Kennedy
Nanomaterials 2024, 14(2), 198; https://doi.org/10.3390/nano14020198 - 16 Jan 2024
Viewed by 718
Abstract
Manganese oxide nanoparticles (MnOx NPs) are finding applications in several environmentally important areas such as farming and energy storage. MnOx NPs span a range of metal oxidation states that open up a wide range of applications in catalysis as well. As [...] Read more.
Manganese oxide nanoparticles (MnOx NPs) are finding applications in several environmentally important areas such as farming and energy storage. MnOx NPs span a range of metal oxidation states that open up a wide range of applications in catalysis as well. As a result, it is important to understand how such materials can impact human health through incidental exposure. In this study, we examined a range of commercially available Mn2O3 NPs and compared our characterization data to those supplied by manufacturers. Discrepancies were noted and then measured values were used to assess the biological impact of these materials on three mammalian cell lines—A549, HepG2 and J774A.1 cells. Cell toxicity assays showed that all Mn2O3 particles exhibited cytotoxic effects that may be correlated, at least in part, to the production of reactive oxygen species. All eight nanoforms also activated caspase 3 but not caspase 1, although the magnitude of these changes varied greatly between materials. Full article
(This article belongs to the Special Issue Advanced Characterization Techniques for Nanomaterials)
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12 pages, 1510 KiB  
Article
Intermixing of Unoccupied States of Metal Phthalocyanine Chains Assembled on Au(110)
by Abhishek Kumar, Maria Grazia Betti, Carlo Mariani, Manvendra Kumar, Pierluigi Gargiani, Cristian Soncini and Maddalena Pedio
Nanomaterials 2024, 14(2), 158; https://doi.org/10.3390/nano14020158 - 11 Jan 2024
Viewed by 665
Abstract
A detailed inverse photoemission study unveils the unoccupied electronic structure induced by the adsorption of CuPc and CoPc phthalocyanines on Au(110) reconstructed channels. The different behavior in the two systems is related to the different intermixing of orbitals with the underlying gold states. [...] Read more.
A detailed inverse photoemission study unveils the unoccupied electronic structure induced by the adsorption of CuPc and CoPc phthalocyanines on Au(110) reconstructed channels. The different behavior in the two systems is related to the different intermixing of orbitals with the underlying gold states. Broadening of the density of states at the Fermi level is detected after CoPc adsorption, absent in the case CuPc. A detailed comparison with the element-selective X-ray absorption spectroscopy enlightens and complements the IPES results and confirms a surface-driven intermixing of the CoPc orbitals involved in the interaction, with the out-of-plane Co 3dz2 orbital strongly hybridized with the gold electronic states. Moreover, the contribution of the 3d empty states to the IPES data is reported for FePc, CoPc, and CuPc thin films. Full article
(This article belongs to the Special Issue Advanced Characterization Techniques for Nanomaterials)
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21 pages, 9676 KiB  
Article
Ti3C2-MXene/NiO Nanocomposites-Decorated CsPbI3 Perovskite Active Materials under UV-Light Irradiation for the Enhancement of Crystal-Violet Dye Photodegradation
by Asma A. Alothman, Mohammad Rizwan Khan, Munirah D. Albaqami, Sonaimuthu Mohandoss, Zeid A. Alothman, Naushad Ahmad and Khadraa N. Alqahtani
Nanomaterials 2023, 13(23), 3026; https://doi.org/10.3390/nano13233026 - 27 Nov 2023
Cited by 4 | Viewed by 1334
Abstract
Ti3C2-MXene material, known for its strong electronic conductivity and optical properties, has emerged as a promising alternative to noble metals as a cocatalyst for the development of efficient photocatalysts used in environmental cleanup. In this study, we investigated the [...] Read more.
Ti3C2-MXene material, known for its strong electronic conductivity and optical properties, has emerged as a promising alternative to noble metals as a cocatalyst for the development of efficient photocatalysts used in environmental cleanup. In this study, we investigated the photodegradation of crystal-violet (CV) dye when exposed to UV light using a newly developed photocatalyst known as Ti3C2-MXene/NiO nanocomposite-decorated CsPbI3 perovskite, which was synthesized through a hydrothermal method. Our research investigation into the structural, morphological, and optical characteristics of the Ti3C2-MXene/NiO/CsPbI3 composite using techniques such as FTIR, XRD, TEM, SEM–EDS mapping, XPS, UV–Vis, and PL spectroscopy. The photocatalytic efficacy of the Ti3C2-MXene/NiO/CsPbI3 composite was assessed by evaluating its ability to degrade CV dye in an aqueous solution under UV-light irradiation. Remarkably, the Ti3C2-MXene/NiO/CsPbI3 composite displayed a significant improvement in both the degradation rate and stability of CV dye when compared to the Ti3C2-MXene/NiO nanocomposite and CsPbI3 perovskite materials. Furthermore, the UV–visible absorption spectrum of the Ti3C2-MXene/NiO/CsPbI3 composite demonstrated a reduced band gap of 2.41 eV, which is lower than that of Ti3C2-MXene/NiO (3.10 eV) and Ti3C2-MXene (1.60 eV). In practical terms, the Ti3C2-MXene/NiO/CsPbI3 composite achieved an impressive 92.8% degradation of CV dye within 90 min of UV light exposure. We also confirmed the significant role of photogenerated holes and radicals in the CV dye removal process through radical scavenger trapping experiments. Based on our findings, we proposed a plausible photocatalytic mechanism for the Ti3C2-MXene/NiO/CsPbI3 composite. This research may open up new avenues for the development of cost-effective and high-performance MXene-based perovskite photocatalysts, utilizing abundant and sustainable materials for environmental remediation. Full article
(This article belongs to the Special Issue Advanced Characterization Techniques for Nanomaterials)
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9 pages, 2061 KiB  
Communication
Exploring TEM Coherence Properties via Speckle Contrast Analysis in Coherent Electron Scattering of Amorphous Material
by Ji-Hwan Kwon, Joohyun Lee, Je In Lee, Byeong-Gwan Cho and Sooheyong Lee
Nanomaterials 2023, 13(23), 3016; https://doi.org/10.3390/nano13233016 - 24 Nov 2023
Viewed by 1002
Abstract
We investigate the coherence properties of a transmission electron microscope by analyzing nano-diffraction speckles originating from bulk metallic glass. The spatial correlation function of the coherent diffraction patterns, obtained in the transmission geometry, reveals the highly coherent nature of the electron probe beam [...] Read more.
We investigate the coherence properties of a transmission electron microscope by analyzing nano-diffraction speckles originating from bulk metallic glass. The spatial correlation function of the coherent diffraction patterns, obtained in the transmission geometry, reveals the highly coherent nature of the electron probe beam and its spatial dimension incident on the sample. Quantitative agreement between the measured speckle contrast and an analytical model yields estimates for the transverse and longitudinal coherence lengths of the source. We also demonstrate that the coherence can be controlled by changing the beam convergence angle. Our findings underscore the preservation of electron beam coherence throughout the electron optics, as evidenced by the high-contrast speckles observed in the scattering patterns of the amorphous system. This study paves the way for the application of advanced coherent diffraction methodologies to investigate local structures and dynamics occurring at atomic-length scales across a diverse range of materials. Full article
(This article belongs to the Special Issue Advanced Characterization Techniques for Nanomaterials)
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13 pages, 3602 KiB  
Article
The Real-Time Monitoring of the Laser-Induced Functionalization of Transparent Conductive Oxide Films
by Takuya Hosokai and Junichi Nomoto
Nanomaterials 2023, 13(19), 2706; https://doi.org/10.3390/nano13192706 - 5 Oct 2023
Viewed by 867
Abstract
Laser-induced functionalization using excimer laser irradiation has been widely applied to transparent conductive oxide films. However, exploring suitable irradiation conditions is time-consuming and cost-ineffective as there are numerous routine film fabrication and analytical processes. Thus, we herein explored a real-time monitoring technique of [...] Read more.
Laser-induced functionalization using excimer laser irradiation has been widely applied to transparent conductive oxide films. However, exploring suitable irradiation conditions is time-consuming and cost-ineffective as there are numerous routine film fabrication and analytical processes. Thus, we herein explored a real-time monitoring technique of the laser-induced functionalization of transparent conductive oxide films. We developed two types of monitoring apparatus, electrical and optical, and applied them to magnetron-sputtered, Sn-doped In2O3 films grown on glass substrates and hydrogen-doped In2O3 films on glass or plastic substrates using a picosecond Nd:YAG pulsed laser. Both techniques could monitor the functionalization from a change in the properties of the films on glass substrates via laser irradiation, but electrical measurement was unsuitable for the plastic samples because of a laser-induced degradation of the underlying plastic substrate, which harmed proper electrical contact. Instead, we proposed that the optical properties in the near-infrared region are more suitable for monitoring. The changes in the optical properties were successfully detected visually in real-time by using an InGaAs near-infrared camera. Full article
(This article belongs to the Special Issue Advanced Characterization Techniques for Nanomaterials)
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23 pages, 6471 KiB  
Article
Quantitative Elasticity Mapping of Submicron Silica Hollow Particles by PeakForce QNM AFM Mode
by Dmitry R. Streltsov, Kirill M. Borisov, Aleksandra A. Kalinina and Aziz M. Muzafarov
Nanomaterials 2023, 13(13), 1916; https://doi.org/10.3390/nano13131916 - 23 Jun 2023
Viewed by 1192
Abstract
Silica hollow spheres with a diameter of 100–300 nm and a shell thickness of 8±2 nm were synthesized using a self-templating amphiphilic polymeric precursor, i.e., poly(ethylene glycol)-substituted hyperbranched polyethoxysiloxane. Their elastic properties were addressed with a high-frequency AFM indentation method based [...] Read more.
Silica hollow spheres with a diameter of 100–300 nm and a shell thickness of 8±2 nm were synthesized using a self-templating amphiphilic polymeric precursor, i.e., poly(ethylene glycol)-substituted hyperbranched polyethoxysiloxane. Their elastic properties were addressed with a high-frequency AFM indentation method based on the PeakForce QNM (quantitative nanomechanical mapping) mode enabling simultaneous visualization of the surface morphology and high-resolution mapping of the mechanical properties. The factors affecting the accuracy of the mechanical measurements such as a local slope of the particle surface, deformation of the silica hollow particles by a solid substrate, shell thickness variation, and applied force range were analysed. The Young’s modulus of the shell material was evaluated as E=26±7 GPa independent of the applied force in the elastic regime of deformations. Beyond the elastic regime, the buckling instability was observed revealing a non-linear force–deformation response with a hysteresis between the loading and unloading force–distance curves and irreversible deformation of the shell at high applied forces. Thus, it was demonstrated that PeakForce QNM mode can be used for quantitative measurements of the elastic properties of submicon-sized silica hollow particles with nano-size shell thickness, as well as for estimation of the buckling behaviour beyond the elastic regime of shell deformations. Full article
(This article belongs to the Special Issue Advanced Characterization Techniques for Nanomaterials)
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