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Nanomaterials
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Characterization of Nanomaterials: Selected Papers from E-MRS Fall 2020
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Characterization of Nanomaterials: Selected Papers from E-MRS Fall 2020

A special issue of Nanomaterials (ISSN 2079-4991).

Deadline for manuscript submissions: closed (15 December 2021) | Viewed by 18440

Special Issue Editors

Prof. Dr. Ehrenfried Zschech

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Guest Editor
Fraunhofer Institute for Ceramic Technologies and Systems, Microelectronic Materials and Nanoanalysis, Dresden, Germany
Interests: functional nanomaterials; nanotechnologies; materials analysis; electronic materials; reliability
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Rodrigo Martins

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Guest Editor
1. Department of Materials Science, School of Science and Technology, NOVA University of Lisbon, 2829-516 Caparica, Portugal
2. Centre of Excellence in Microelectronics and Optoelectronics Processes of the Institute of New Technologies, CEMOP/UNINOVA, 2829-516 Caparica, Portugal
Interests: functional nanomaterials; paper electronics; advanced functional materials; thin film solar cells; nanotechnologies
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Eva Olsson

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Guest Editor
Chalmers University of Technology, Department of Physics, Göteborg, Sweden
Interests: advanced electron microscopy; in-situ techniques; advanced functional nanomaterials
Prof. Dr. Sabrina Sartori

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Guest Editor
Department of Physics, University of Oslo, Oslo, Norway
Interests: nano-scale materials; spectroscopy; neutron scattering; materials for energy storage and conversion
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Prof. Dr. Robert Sinclair

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Guest Editor
Stanford University, USA Stanford University, Department of Materials Science and Engineering, Stanford/CA, USA
Interests: advanced and in-situ electron microscopy; material reactions; thin film structures; energy materials; nanotechnology for cancer detection
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

The characterization of nanomaterials is of great scientific interest and increasing industrial relevance, particularly for applications to high-tech products. This Special Issue of Nanomaterials, “Characterization of Nanomaterials”, aims to cover a broad range of subjects in the field of nanoanalysis and material characterization along the whole value and innovation chain. It focuses on the development and application of microscopy, spectroscopy and diffraction techniques. New findings relating to disruptive nanoanalysis techniques will be reported, and novel solutions in the field of material characterization for process and quality control will be presented. This Special Issue will include original research papers and comprehensive review articles covering the most recent progress and new developments in the nano-scale characterization of materials.

The papers in this Special Issue will be based on selected presentations at the web-based E-MRS European Nanoanalysis Symposium held on October 9, 2020. The symposium will bring together scientists and engineers from universities, research institutions, equipment manufacturers and industrial end-users. The discussions between the stakeholders will help to identify gaps in the fields of advancing nanoanalysis and material characterization and to propose actions to close them and to support the industrial exploitation of innovative materials.

Prof. Dr. Ehrenfried Zschech
Prof. Dr. Rodrigo Martins
Prof. Dr. Eva Olsson
Prof. Dr. Sabrina Sartori
Prof. Dr. Robert Sinclair
Guest Editors

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

  • material characterization
  • nanoanalysis
  • electron microscopy
  • X-ray microscopy
  • nanomechanics
  • spectroscopy
  • diffraction.

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Published Papers (6 papers)

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Research

11 pages, 3227 KiB  
Article
Monitored Tomographic Reconstruction—An Advanced Tool to Study the 3D Morphology of Nanomaterials
by Konstantin Bulatov, Marina Chukalina, Kristina Kutukova, Vlad Kohan, Anastasia Ingacheva, Alexey Buzmakov, Vladimir V. Arlazarov and Ehrenfried Zschech
Nanomaterials 2021, 11(10), 2524; https://doi.org/10.3390/nano11102524 - 27 Sep 2021
Cited by 6 | Viewed by 2140
Abstract
Detailed and accurate three-dimensional (3D) information about the morphology of hierarchically structured materials is derived from multi-scale X-ray computed tomography (XCT) and subsequent 3D data reconstruction. High-resolution X-ray microscopy and nano-XCT are suitable techniques to nondestructively study nanomaterials, including porous or skeleton materials. [...] Read more.
Detailed and accurate three-dimensional (3D) information about the morphology of hierarchically structured materials is derived from multi-scale X-ray computed tomography (XCT) and subsequent 3D data reconstruction. High-resolution X-ray microscopy and nano-XCT are suitable techniques to nondestructively study nanomaterials, including porous or skeleton materials. However, laboratory nano-XCT studies are very time-consuming. To reduce the time-to-data by more than an order of magnitude, we propose taking advantage of a monitored tomographic reconstruction. The benefit of this new protocol for 3D imaging is that the data acquisition for each projection is interspersed by image reconstruction. We demonstrate this new approach for nano-XCT data of a novel transition-metal-based materials system: MoNi4 electrocatalysts anchored on MoO2 cuboids aligned on Ni foam (MoNi4/MoO2@Ni). Quantitative data that describe the 3D morphology of this hierarchically structured system with an advanced electrocatalytically active nanomaterial are needed to tailor performance and durability of the electrocatalyst system. We present the framework for monitored tomographic reconstruction, construct three stopping rules for various reconstruction quality metrics and provide their experimental evaluation. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from E-MRS Fall 2020)
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14 pages, 2965 KiB  
Article
Optical Monitoring of the Biodegradation of Porous and Solid Silicon Nanoparticles
by Maxim B. Gongalsky, Nikolay V. Pervushin, Daria E. Maksutova, Uliana A. Tsurikova, Pavel P. Putintsev, Oleg D. Gyuppenen, Yana V. Evstratova, Olga A. Shalygina, Gelina S. Kopeina, Andrey A. Kudryavtsev, Boris Zhivotovsky and Liubov A. Osminkina
Nanomaterials 2021, 11(9), 2167; https://doi.org/10.3390/nano11092167 - 25 Aug 2021
Cited by 10 | Viewed by 3370
Abstract
Silicon nanoparticles (SiNP) are currently of great interest, especially in biomedicine, because of their unique physicochemical properties combined with biodegradability. SiNPs can be obtained in various ways and can have either a non-porous solid (sol-) or porous (por-) structure. In this work, we [...] Read more.
Silicon nanoparticles (SiNP) are currently of great interest, especially in biomedicine, because of their unique physicochemical properties combined with biodegradability. SiNPs can be obtained in various ways and can have either a non-porous solid (sol-) or porous (por-) structure. In this work, we carry out detailed optical monitoring of sol- and por-SiNP biodegradation using Raman and photoluminescence (PL) micro-spectroscopy. SiNPs were obtained by ultrasound grinding of sol- or por-silicon nanowires, created by silver-assisted chemical etching of crystalline Si with different doping levels. In this case, sol-SiNPs consist of nanocrystals 30 nm in size, while por-SiNPs consist of small 3 nm nanocrystals and 16 nm pores. Both SiNPs show low in vitro cytotoxicity towards MCF-7 and HEK293T cells up to 800 μg/mL. The appearance of the F-band (blue–yellow) PL, as well as a decrease in the intensity of the Raman signal, indicate the gradual dissolution of the sol-SiNPs during 20 days of incubation. At the same time, the rapid dissolution of por-SiNP within 24 h is identified by the quenching of their S-band (red) PL and the disappearance of the Raman signal. The obtained results are important for development of intelligent biodegradable drug delivery systems based on SiNPs. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from E-MRS Fall 2020)
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12 pages, 13680 KiB  
Article
Morphology and Mechanical Properties of Fossil Diatom Frustules from Genera of Ellerbeckia and Melosira
by Qiong Li, Jürgen Gluch, Zhongquan Liao, Juliane Posseckardt, André Clausner, Magdalena Łępicka, Małgorzata Grądzka-Dahlke and Ehrenfried Zschech
Nanomaterials 2021, 11(6), 1615; https://doi.org/10.3390/nano11061615 - 20 Jun 2021
Viewed by 2639
Abstract
Fossil frustules of Ellerbeckia and Melosira were studied using laboratory-based nano X-ray tomography (nano-XCT), transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDS). Three-dimensional (3D) morphology characterization using nondestructive nano-XCT reveals the continuous connection of fultoportulae, tube processes and protrusions. The study confirms [...] Read more.
Fossil frustules of Ellerbeckia and Melosira were studied using laboratory-based nano X-ray tomography (nano-XCT), transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDS). Three-dimensional (3D) morphology characterization using nondestructive nano-XCT reveals the continuous connection of fultoportulae, tube processes and protrusions. The study confirms that Ellerbeckia is different from Melosira. Both genera reveal heavily silicified frustules with valve faces linking together and forming cylindrical chains. For this cylindrical architecture of both genera, valve face thickness, mantle wall thickness and copulae thickness change with the cylindrical diameter. Furthermore, EDS reveals that these fossil frustules contain Si and O only, with no other elements in the percentage concentration range. Nanopores with a diameter of approximately 15 nm were detected inside the biosilica of both genera using TEM. In situ micromechanical experiments with uniaxial loading were carried out within the nano-XCT on these fossil frustules to determine the maximal loading force under compression and to describe the fracture behavior. The fracture force of both genera is correlated to the dimension of the fossil frustules. The results from in situ mechanical tests show that the crack initiation starts either at very thin features or at linking structures of the frustules. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from E-MRS Fall 2020)
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16 pages, 3167 KiB  
Article
Atomic Level Insight into Wetting and Structure of Ag Droplet on Graphene Coated Copper Substrate—Molecular Dynamics versus Experiment
by Aleksandra Drewienkiewicz, Arkadiusz Żydek, Marcela E. Trybula and Janusz Pstruś
Nanomaterials 2021, 11(6), 1465; https://doi.org/10.3390/nano11061465 - 1 Jun 2021
Cited by 8 | Viewed by 3094
Abstract
Understanding the atomic-level phenomena occurring upon the wetting of graphene-coated Cu with liquid Ag is pivotal for the description of the wetting phenomenon and the role of graphene as a diffusion barrier. We have performed molecular dynamics (MD) simulations and confronted with our [...] Read more.
Understanding the atomic-level phenomena occurring upon the wetting of graphene-coated Cu with liquid Ag is pivotal for the description of the wetting phenomenon and the role of graphene as a diffusion barrier. We have performed molecular dynamics (MD) simulations and confronted with our present experimental results to characterize wetting behavior of graphene coated Cu surfaces. Perfect and defected graphene layers covering Cu surface were wetted with liquid Ag droplet at 1273 K. Structural and topological aspects are discussed to characterize structure of the liquid Ag droplet and a product of wetting reaction occurring on Cu/Gn and Cu/Gndef substrates, also including perfect graphene layer and a pure Cu surface. The obtained results reveal the importance of defects in graphene structure, which play a key role in wetting mechanism and the formation of AgCu alloy. As a consequence, we observe a change of the wetting behavior and topology of both bulk and adsorbed Ag atoms by using Voronoi analysis (VA). Despite the differences in time scale, atomistic simulations allowed us to catch the early stages of wetting, which are important for explaining the final stage of wetting delivered from experiment. Our findings reveal also graphene translucency to metal-metal interactions, observed in previous papers. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from E-MRS Fall 2020)
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13 pages, 5760 KiB  
Article
Microstructure and Fracture Mechanism Investigation of Porous Silicon Nitride–Zirconia–Graphene Composite Using Multi-Scale and In-Situ Microscopy
by Zhongquan Liao, Yvonne Standke, Jürgen Gluch, Katalin Balázsi, Onkar Pathak, Sören Höhn, Mathias Herrmann, Stephan Werner, Ján Dusza, Csaba Balázsi and Ehrenfried Zschech
Nanomaterials 2021, 11(2), 285; https://doi.org/10.3390/nano11020285 - 22 Jan 2021
Cited by 4 | Viewed by 3155
Abstract
Silicon nitride–zirconia–graphene composites with high graphene content (5 wt.% and 30 wt.%) were sintered by gas pressure sintering (GPS). The effect of the multilayer graphene (MLG) content on microstructure and fracture mechanism is investigated by multi-scale and in-situ microscopy. Multi-scale microscopy confirms that [...] Read more.
Silicon nitride–zirconia–graphene composites with high graphene content (5 wt.% and 30 wt.%) were sintered by gas pressure sintering (GPS). The effect of the multilayer graphene (MLG) content on microstructure and fracture mechanism is investigated by multi-scale and in-situ microscopy. Multi-scale microscopy confirms that the phases disperse evenly in the microstructure without obvious agglomeration. The MLG flakes well dispersed between ceramic matrix grains slow down the phase transformation from α to β-Si3N4, subsequent needle-like growth of β-Si3N4 rods and the densification due to the reduction in sintering additives particularly in the case with 30 wt.% MLG. The size distribution of Si3N4 phase shifts towards a larger size range with the increase in graphene content from 5 to 30 wt.%, while a higher graphene content (30 wt.%) hinders the growth of the ZrO2 phase. The composite with 30 wt.% MLG has a porosity of 47%, the one with 5 wt.% exhibits a porosity of approximately 30%. Both Si3N4/MLG composites show potential resistance to contact or indentation damage. Crack initiation and propagation, densification of the porous microstructure, and shift of ceramic phases are observed using in-situ transmission electron microscopy. The crack propagates through the ceramic/MLG interface and through both the ceramic and the non-ceramic components in the composite with low graphene content. However, the crack prefers to bypass ceramic phases in the composite with 30 wt.% MLG. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from E-MRS Fall 2020)
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13 pages, 2304 KiB  
Article
Laboratory Operando XAS Study of Sodium Iron Titanite Cathode in the Li-Ion Half-Cell
by Victor Shapovalov, Alexander Guda, Vera Butova, Igor Shukaev and Alexander Soldatov
Nanomaterials 2021, 11(1), 156; https://doi.org/10.3390/nano11010156 - 9 Jan 2021
Cited by 9 | Viewed by 2729
Abstract
Electrochemical characterization of the novel sodium iron titanate Na0.9Fe0.45Ti1.55O4 was performed upon cycling in the Li-ion half-cell. The material exhibited stable cycling in the voltage range 2–4.5 V, and the number of alkali ions extracted per [...] Read more.
Electrochemical characterization of the novel sodium iron titanate Na0.9Fe0.45Ti1.55O4 was performed upon cycling in the Li-ion half-cell. The material exhibited stable cycling in the voltage range 2–4.5 V, and the number of alkali ions extracted per formula unit was approximately half of the Na stoichiometry value. Using laboratory X-ray absorption spectrometry, we measured operando Fe K-edge X-ray absorption spectra in the first 10 charge–discharge cycles and quantified the portion of charge associated with the transition metal redox reaction. Although 3d metals are commonly accepted redox-active centers in the intercalation process, we found that in all cycles the amount of oxidized and reduced Fe ions was almost 20% less than the total number of transferred electrons. Using density functional theory (DFT) simulations, we show that part of the reversible capacity is related to the redox reaction on oxygen ions. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from E-MRS Fall 2020)
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