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Nanomaterials
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Characterization of Nanomaterials
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Characterization of Nanomaterials

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

Deadline for manuscript submissions: closed (31 March 2020) | Viewed by 29006

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. 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
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. Marco Sebastiani

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Guest Editor
Università degli studi Roma Tre, Roma, Italy
Interests: nanoindentation; FIB; residual stress; thin films; fracture; nanomechanics
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Olivier Thomas

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Guest Editor
Aix-Marseille University, CNRS, Institute Materials Microelectronics and Nanoscience, Marseille, France
Interests: nanomechanics; materials for microelectronics; materials characterization; X-ray diffraction; in-situ experiments; synchrotron radiation

Special Issue Information

Dear Colleagues,

The characterization of nanomaterials is of significant scientific interest and increasing industrial relevance, particularly for high-tech product applications. This Special Issue of Nanomaterials, “Characterization of Nanomaterials”, aims to cover a broad range of subjects in the field of nanoanalysis and materials characterization, along the entirety of the value and innovation chain. The primary focus of this Special Issue is the development and application of microscopy, spectroscopy and diffraction techniques. New research results in disruptive nanoanalysis techniques will be reported, and novel solutions in the field of materials characterization for process and quality control will be shown. This special issue will include original research articles and comprehensive review articles covering recent progress and new developments in the nano-scale characterization of materials.

The papers in this Special Issue are based on selected presentations from the 7th Dresden Nanoanalysis Symposium, held in Dresden on 30 August 2019. It brought together scientists and engineers from universities, research institutions, equipment manufacturers and industrial end-users. The discussions and interactions between the stakeholders helped identify gaps in the advancing fields of nanoanalysis and materials characterization, and to propose actions to close the gaps and support industrial exploitation of innovative materials.

Prof. Dr. Ehrenfried Zschech
Prof. Dr. Robert Sinclair
Prof. Dr. Rodrigo Martins
Prof. Dr. Marco Sebastiani
Prof. Dr. Olivier Thomas
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

  • materials characterization
  • nanoanalysis
  • electron microscopy
  • X-ray microscopy
  • nanomechanics
  • spectroscopy
  • diffraction

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Published Papers (7 papers)

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Research

8 pages, 1226 KiB  
Article
Stress Buildup Upon Crystallization of GeTe Thin Films: Curvature Measurements and Modelling
by Rajkiran Tholapi, Manon Gallard, Nelly Burle, Christophe Guichet, Stephanie Escoubas, Magali Putero, Cristian Mocuta, Marie-Ingrid Richard, Rebecca Chahine, Chiara Sabbione, Mathieu Bernard, Leila Fellouh, Pierre Noé and Olivier Thomas
Nanomaterials 2020, 10(6), 1247; https://doi.org/10.3390/nano10061247 - 26 Jun 2020
Cited by 2 | Viewed by 2920
Abstract
Phase change materials are attractive materials for non-volatile memories because of their ability to switch reversibly between an amorphous and a crystal phase. The volume change upon crystallization induces mechanical stress that needs to be understood and controlled. In this work, we monitor [...] Read more.
Phase change materials are attractive materials for non-volatile memories because of their ability to switch reversibly between an amorphous and a crystal phase. The volume change upon crystallization induces mechanical stress that needs to be understood and controlled. In this work, we monitor stress evolution during crystallization in thin GeTe films capped with SiOx, using optical curvature measurements. A 150 MPa tensile stress buildup is measured when the 100 nm thick film crystallizes. Stress evolution is a result of viscosity increase with time and a tentative model is proposed that renders qualitatively the observed features. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials)
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17 pages, 3443 KiB  
Article
Polyelectrolyte Multilayer Films Modification with Ag and rGO Influences Platelets Activation and Aggregate Formation under In Vitro Blood Flow
by Gabriela Imbir, Aldona Mzyk, Klaudia Trembecka-Wójciga, Ewa Jasek-Gajda, Hanna Plutecka, Romana Schirhagl and Roman Major
Nanomaterials 2020, 10(5), 859; https://doi.org/10.3390/nano10050859 - 29 Apr 2020
Cited by 8 | Viewed by 2847
Abstract
Surface functionalization of materials to improve their hemocompatibility is a challenging problem in the field of blood-contacting devices and implants. Polyelectrolyte multilayer films (PEMs), which can mimic functions and structure of an extracellular matrix (ECM), are a promising solution to the urgent need [...] Read more.
Surface functionalization of materials to improve their hemocompatibility is a challenging problem in the field of blood-contacting devices and implants. Polyelectrolyte multilayer films (PEMs), which can mimic functions and structure of an extracellular matrix (ECM), are a promising solution to the urgent need for functional blood-contacting coatings. The properties of PEMs can be easily tuned in order to provide a scaffold with desired physico-chemical parameters. In this study chitosan/chondroitin sulfate (Chi/CS) polyelectrolyte multilayers were deposited on medical polyurethane. Afterwards PEMs were modified by chemical cross-linking and nanoparticles introduction. Coatings with variable properties were tested for their hemocompatibility in the cone-plate tester under dynamic conditions. The obtained results enable the understanding of how substrate properties modulate PEMs interaction with blood plasma proteins and the morphotic elements. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials)
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16 pages, 8458 KiB  
Article
Nano-Scale Residual Stress Profiling in Thin Multilayer Films with Non-Equibiaxial Stress State
by Marco Sebastiani, Edoardo Rossi, Muhammad Zeeshan Mughal, Alessandro Benedetto, Paul Jacquet, Enrico Salvati and Alexander M. Korsunsky
Nanomaterials 2020, 10(5), 853; https://doi.org/10.3390/nano10050853 - 28 Apr 2020
Cited by 17 | Viewed by 4705
Abstract
Silver-based low-emissivity (low-E) coatings are applied on architectural glazing to cost-effectively reduce heat losses, as they generally consist of dielectric/Ag/dielectric multilayer stacks, where the thin Ag layer reflects long- wavelength infrared (IR), while the dielectric layers both protect the Ag and act as [...] Read more.
Silver-based low-emissivity (low-E) coatings are applied on architectural glazing to cost-effectively reduce heat losses, as they generally consist of dielectric/Ag/dielectric multilayer stacks, where the thin Ag layer reflects long- wavelength infrared (IR), while the dielectric layers both protect the Ag and act as an anti-reflective barrier. The architecture of the multilayer stack influences its mechanical properties and it is strongly dependent on the residual stress distribution in the stack. Residual stress evaluation by combining focused ion beam (FIB) milling and digital image correlation (DIC), using the micro-ring core configuration (FIB-DIC), offers micron-scale lateral resolution and provides information about the residual stress variation with depth, i.e., it allows depth profiling for both equibiaxial and non-equibiaxial stress distributions and hence can be effectively used to characterize low-E coatings. In this work, we propose an innovative approach to improve the depth resolution and surface sensitivity for residual stress depth profiling in the case of ultra-thin as-deposited and post-deposition annealed Si3N4/Ag/ZnO low-E coatings, by considering different fractions of area for DIC strain analysis and accordingly developing a unique influence function to maintain the sensitivity of the technique at is maximum during the calculation. Residual stress measurements performed using this novel FIB-DIC approach revealed that the individual Si3N4/ZnO layers in the multilayer stack are under different amounts of compressive stresses. The magnitude and orientation of these stresses changes significantly after heat treatment and provides a clear explanation for the observed differences in terms of scratch critical load. The results show that the proposed FIB-DIC combined-areas approach is a unique method for accurately probing non-equibiaxial residual stresses with nano-scale resolution in thin films, including multilayers. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials)
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26 pages, 6530 KiB  
Article
Testing Novel Portland Cement Formulations with Carbon Nanotubes and Intrinsic Properties Revelation: Nanoindentation Analysis with Machine Learning on Microstructure Identification
by Georgios Konstantopoulos, Elias P. Koumoulos and Costas A. Charitidis
Nanomaterials 2020, 10(4), 645; https://doi.org/10.3390/nano10040645 - 30 Mar 2020
Cited by 33 | Viewed by 4303
Abstract
Nanoindentation was utilized as a non-destructive technique to identify Portland Cement hydration phases. Artificial Intelligence (AI) and semi-supervised Machine Learning (ML) were used for knowledge gain on the effect of carbon nanotubes to nanomechanics in novel cement formulations. Data labelling is performed with [...] Read more.
Nanoindentation was utilized as a non-destructive technique to identify Portland Cement hydration phases. Artificial Intelligence (AI) and semi-supervised Machine Learning (ML) were used for knowledge gain on the effect of carbon nanotubes to nanomechanics in novel cement formulations. Data labelling is performed with unsupervised ML with k-means clustering. Supervised ML classification is used in order to predict the hydration products composition and 97.6% accuracy was achieved. Analysis included multiple nanoindentation raw data variables, and required less time to execute than conventional single component probability density analysis (PDA). Also, PDA was less informative than ML regarding information exchange and re-usability of input in design predictions. In principle, ML is the appropriate science for predictive modeling, such as cement phase identification and facilitates the acquisition of precise results. This study introduces unbiased structure-property relations with ML to monitor cement durability based on cement phases nanomechanics compared to PDA, which offers a solution based on local optima of a multidimensional space solution. Evaluation of nanomaterials inclusion in composite reinforcement using semi-supervised ML was proved feasible. This methodology is expected to contribute to design informatics due to the high prediction metrics, which holds promise for the transfer learning potential of these models for studying other novel cement formulations. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials)
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12 pages, 6547 KiB  
Article
Anisotropy of Mechanical Properties of Pinctada margaritifera Mollusk Shell
by Martyna Strąg, Łukasz Maj, Magdalena Bieda, Paweł Petrzak, Anna Jarzębska, Jürgen Gluch, Emre Topal, Kristina Kutukova, André Clausner, Wieland Heyn, Katarzyna Berent, Kinga Nalepka, Ehrenfried Zschech, Antonio G. Checa and Krzysztof Sztwiertnia
Nanomaterials 2020, 10(4), 634; https://doi.org/10.3390/nano10040634 - 28 Mar 2020
Cited by 17 | Viewed by 3641
Abstract
The mechanical properties such as compressive strength and nanohardness were investigated for Pinctada margaritifera mollusk shells. The compressive strength was evaluated through a uniaxial static compression test performed along the load directions parallel and perpendicular to the shell axis, respectively, while the hardness [...] Read more.
The mechanical properties such as compressive strength and nanohardness were investigated for Pinctada margaritifera mollusk shells. The compressive strength was evaluated through a uniaxial static compression test performed along the load directions parallel and perpendicular to the shell axis, respectively, while the hardness and Young modulus were measured using nanoindentation. In order to observe the crack propagation, for the first time for such material, the in-situ X-ray microscopy (nano-XCT) imaging (together with 3D reconstruction based on the acquired images) during the indentation tests was performed. The results were compared with these obtained during the micro-indentation test done with the help of conventional Vickers indenter and subsequent scanning electron microscopy observations. The results revealed that the cracks formed during the indentation start to propagate in the calcite prism until they reach a ductile organic matrix where most of them are stopped. The obtained results confirm a strong anisotropy of both crack propagation and the mechanical strength caused by the formation of the prismatic structure in the outer layer of P. margaritifera shell. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials)
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11 pages, 3078 KiB  
Article
Structural and Electrical Comparison of Si and Zr Doped Hafnium Oxide Thin Films and Integrated FeFETs Utilizing Transmission Kikuchi Diffraction
by Maximilian Lederer, Thomas Kämpfe, Norman Vogel, Dirk Utess, Beate Volkmann, Tarek Ali, Ricardo Olivo, Johannes Müller, Sven Beyer, Martin Trentzsch, Konrad Seidel and Lukas M. Eng
Nanomaterials 2020, 10(2), 384; https://doi.org/10.3390/nano10020384 - 22 Feb 2020
Cited by 53 | Viewed by 6089
Abstract
The microstructure of ferroelectric hafnium oxide plays a vital role for its application, e.g., non-volatile memories. In this study, transmission Kikuchi diffraction and scanning transmission electron microscopy STEM techniques are used to compare the crystallographic phase and orientation of Si and Zr doped [...] Read more.
The microstructure of ferroelectric hafnium oxide plays a vital role for its application, e.g., non-volatile memories. In this study, transmission Kikuchi diffraction and scanning transmission electron microscopy STEM techniques are used to compare the crystallographic phase and orientation of Si and Zr doped HfO2 thin films as well as integrated in a 22 nm fully-depleted silicon-on-insulator (FDSOI) ferroelectric field effect transistor (FeFET). Both HfO2 films showed a predominately orthorhombic phase in accordance with electrical measurements and X-ray diffraction XRD data. Furthermore, a stronger texture is found for the microstructure of the Si doped HfO2 (HSO) thin film, which is attributed to stress conditions inside the film stack during crystallization. For the HSO thin film fabricated in a metal-oxide-semiconductor (MOS) like structure, a different microstructure, with no apparent texture as well as a different fraction of orthorhombic phase is observed. The 22 nm FDSOI FeFET showed an orthorhombic phase for the HSO layer, as well as an out-of-plane texture of the [111]-axis, which is preferable for the application as non-volatile memory. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials)
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11 pages, 1394 KiB  
Article
Nanoscale Estimation of Coating Thickness on Substrates via Standardless BSE Detector Calibration
by Radim Skoupy, Tomas Fort and Vladislav Krzyzanek
Nanomaterials 2020, 10(2), 332; https://doi.org/10.3390/nano10020332 - 15 Feb 2020
Cited by 7 | Viewed by 3584
Abstract
The thickness of electron transparent samples can be measured in an electron microscope using several imaging techniques like electron energy loss spectroscopy (EELS) or quantitative scanning transmission electron microscopy (STEM). We extrapolate this method for using a back-scattered electron (BSE) detector in the [...] Read more.
The thickness of electron transparent samples can be measured in an electron microscope using several imaging techniques like electron energy loss spectroscopy (EELS) or quantitative scanning transmission electron microscopy (STEM). We extrapolate this method for using a back-scattered electron (BSE) detector in the scanning electron microscope (SEM). This brings the opportunity to measure the thickness not just of the electron transparent samples on TEM mesh grids, but, in addition, also the thickness of thin films on substrates. Nevertheless, the geometry of the microscope and the BSE detector poses a problem with precise calibration of the detector. We present a simple method which can be used for such a type of detector calibration that allows absolute (standardless) measurement of thickness, together with a proof of the method on test samples. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials)
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