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Nanomaterials
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Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposiumc
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Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposiumc

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

Deadline for manuscript submissions: closed (31 December 2018) | Viewed by 46446

Printed Edition Available!
A printed edition of this Special Issue is available here.

Special Issue Editors

Prof. Dr. Ehrenfried Zschech

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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
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Prof. Dr. Rodrigo Martins

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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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Università degli studi Roma Tre, Roma, Italy
Interests: nanoindentation; FIB; residual stress; thin films; fracture; nanomechanics
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Prof. Dr. Sabrina Sartori

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Department of Physics, University of Oslo, Oslo, Norway
Interests: nano-scale materials; spectroscopy; neutron scattering; materials for energy storage and conversion
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

The characterization of nanomaterials is of high scientific interest and of 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 materials characterization along the whole value and innovation chain. It focuses on 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 the most recent progress and new developments in the nano-scale characterization of materials.

The papers in this Special Issue are based on selected presentations at the 6th Dresden Nanoanalysis Symposium which was held in Dresden on 31 August 2018. It brought together scientists and engineers from universities, research institutions, equipment manufacturers, and industrial end-users. The discussions and interactions between the stakeholders will help to identify gaps in the fields of advancing nanoanalysis and materials characterization and to propose actions to close them and to support the industrial exploitation of innovative materials.

Prof. Dr. Ehrenfried Zschech
Prof. Dr. Robert Sinclair
Prof. Dr. Rodrigo Martins
Prof. Dr. Marco Sebastiani
Prof. Dr. Sabrina Sartori
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

Published Papers (10 papers)

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Editorial

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4 pages, 175 KiB  
Editorial
Editorial for the Special Issue “Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposium”
by Ehrenfried Zschech, Robert Sinclair, Rodrigo Martins, Marco Sebastiani and Sabrina Sartori
Nanomaterials 2019, 9(11), 1527; https://doi.org/10.3390/nano9111527 - 27 Oct 2019
Viewed by 2379
Abstract
More than ever before, materials-driven product innovations in industry and shorter time-to-market introductions for new products require high advancement rates and a tight coupling between research, development and manufacturing [...] Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposiumc)

Research

Jump to: Editorial

14 pages, 9593 KiB  
Article
ToF-SIMS 3D Analysis of Thin Films Deposited in High Aspect Ratio Structures via Atomic Layer Deposition and Chemical Vapor Deposition
by Alireza M. Kia, Nora Haufe, Sajjad Esmaeili, Clemens Mart, Mikko Utriainen, Riikka L. Puurunen and Wenke Weinreich
Nanomaterials 2019, 9(7), 1035; https://doi.org/10.3390/nano9071035 - 19 Jul 2019
Cited by 19 | Viewed by 7546
Abstract
For the analysis of thin films, with high aspect ratio (HAR) structures, time-of-flight secondary ion mass spectrometry (ToF-SIMS) overcomes several challenges in comparison to other frequently used techniques such as electron microscopy. The research presented herein focuses on two different kinds of HAR [...] Read more.
For the analysis of thin films, with high aspect ratio (HAR) structures, time-of-flight secondary ion mass spectrometry (ToF-SIMS) overcomes several challenges in comparison to other frequently used techniques such as electron microscopy. The research presented herein focuses on two different kinds of HAR structures that represent different semiconductor technologies. In the first study, ToF-SIMS is used to illustrate cobalt seed layer corrosion by the copper electrolyte within the large through-silicon-vias (TSVs) before and after copper electroplating. However, due to the sample’s surface topography, ToF-SIMS analysis proved to be difficult due to the geometrical shadowing effects. Henceforth, in the second study, we introduce a new test platform to eliminate the difficulties with the HAR structures, and again, use ToF-SIMS for elemental analysis. We use data image slicing of 3D ToF-SIMS analysis combined with lateral HAR test chips (PillarHall™) to study the uniformity of silicon dopant concentration in atomic layer deposited (ALD) HfO2 thin films. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposiumc)
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18 pages, 3581 KiB  
Article
Role of Structure and Composition on the Performances of P-Type Tin Oxide Thin-Film Transistors Processed at Low-Temperatures
by Raquel Barros, Kachirayil J. Saji, João C. Waerenborgh, Pedro Barquinha, Luís Pereira, Emanuel Carlos, Rodrigo Martins and Elvira Fortunato
Nanomaterials 2019, 9(3), 320; https://doi.org/10.3390/nano9030320 - 01 Mar 2019
Cited by 30 | Viewed by 4353
Abstract
This work reports on the role of structure and composition on the determination of the performances of p-type SnOx TFTs with a bottom gate configuration deposited by rf magnetron sputtering at room temperature, followed by a post-annealed step up to 200 °C [...] Read more.
This work reports on the role of structure and composition on the determination of the performances of p-type SnOx TFTs with a bottom gate configuration deposited by rf magnetron sputtering at room temperature, followed by a post-annealed step up to 200 °C at different oxygen partial pressures (Opp) between 0% and 20% but where the p-type conduction was only observed between in a narrow window, from 2.8% to 3.8%. The role of structure and composition were evaluated by XRD and Mössbauer spectroscopic studies that allows to identify the best phases/compositions and thicknesses (around 12 nm) to be used to produce p-type TFTs with saturation mobility of 4.6 cm2 V−1 s−1 and on-off ratio above 7 × 104, operating at the enhancement mode with a saturation voltage of −10 V. Moreover, a brief overview is also presented concerning the present state of the existing developments in processing SnOx TFTs with different methods and using different device configurations. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposiumc)
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10 pages, 3264 KiB  
Article
Multi-Level Cell Properties of a Bilayer Cu2O/Al2O3 Resistive Switching Device
by Jonas Deuermeier, Asal Kiazadeh, Andreas Klein, Rodrigo Martins and Elvira Fortunato
Nanomaterials 2019, 9(2), 289; https://doi.org/10.3390/nano9020289 - 19 Feb 2019
Cited by 22 | Viewed by 3773
Abstract
Multi-level resistive switching characteristics of a Cu2O/Al2O3 bilayer device are presented. An oxidation state gradient in copper oxide induced by the fabrication process was found to play a dominant role in defining the multiple resistance states. The highly [...] Read more.
Multi-level resistive switching characteristics of a Cu2O/Al2O3 bilayer device are presented. An oxidation state gradient in copper oxide induced by the fabrication process was found to play a dominant role in defining the multiple resistance states. The highly conductive grain boundaries of the copper oxide—an unusual property for an oxide semiconductor—are discussed for the first time regarding their role in the resistive switching mechanism. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposiumc)
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14 pages, 3317 KiB  
Article
Recovery of Li(Ni0.33Mn0.33Co0.33)O2 from Lithium-Ion Battery Cathodes: Aspects of Degradation
by Tim Sieber, Jana Ducke, Anja Rietig, Thomas Langner and Jörg Acker
Nanomaterials 2019, 9(2), 246; https://doi.org/10.3390/nano9020246 - 12 Feb 2019
Cited by 20 | Viewed by 5807
Abstract
Nickel–manganese–cobalt oxides, with LiNi0.33Mn0.33Co0.33O2 (NMC) as the most prominent compound, are state-of-the-art cathode materials for lithium-ion batteries in electric vehicles. The growing market for electro mobility has led to a growing global demand for Li, Co, [...] Read more.
Nickel–manganese–cobalt oxides, with LiNi0.33Mn0.33Co0.33O2 (NMC) as the most prominent compound, are state-of-the-art cathode materials for lithium-ion batteries in electric vehicles. The growing market for electro mobility has led to a growing global demand for Li, Co, Ni, and Mn, making spent lithium-ion batteries a valuable secondary resource. Going forward, energy- and resource-inefficient pyrometallurgical and hydrometallurgical recycling strategies must be avoided. We presented an approach to recover NMC particles from spent lithium-ion battery cathodes while preserving their chemical and morphological properties, with a minimal use of chemicals. The key task was the separation of the cathode coating layer consisting of NMC, an organic binder, and carbon black, from the Al substrate foil. This can be performed in water under strong agitation to support the slow detachment process. However, the contact of the NMC cathode with water leads to a release of Li+ ions and a fast increase in the pH. Unwanted side reactions may occur as the Al substrate foil starts to dissolve and Al(OH)3 precipitates on the NMC. These side reactions are avoided using pH-adjusted solutions with sufficiently high buffer capacities to separate the coating layer from the Al substrate, without precipitations and without degradation of the NMC particles. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposiumc)
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8 pages, 2479 KiB  
Article
Investigation of the Surface of Ga–Sn–Zn Eutectic Alloy by the Characterisation of Oxide Nanofilms Obtained by the Touch-Printing Method
by Alexandra Dobosz, Torben Daeneke, Ali Zavabeti, Bao Yue Zhang, Rebecca Orrell-Trigg, Kourosh Kalantar-Zadeh, Anna Wójcik, Wojciech Maziarz and Tomasz Gancarz
Nanomaterials 2019, 9(2), 235; https://doi.org/10.3390/nano9020235 - 09 Feb 2019
Cited by 11 | Viewed by 3794
Abstract
Ga–Sn–Zn eutectic alloy is a non-toxic liquid metal alloy which could be used in a multitude of applications, including as a heat transfer agent, in gas sensing, and in medicine. Alloys containing gallium readily oxidise in air, forming a thin oxide layer that [...] Read more.
Ga–Sn–Zn eutectic alloy is a non-toxic liquid metal alloy which could be used in a multitude of applications, including as a heat transfer agent, in gas sensing, and in medicine. Alloys containing gallium readily oxidise in air, forming a thin oxide layer that influences the properties of liquid metals and which has not been studied. In this study, the oxide layer formed on Ga–Sn–Zn alloy was transferred at room temperature onto three substrates—quartz, glass and silicon. The contact angle between the liquid alloy and different substrates was determined. The obtained thin oxide films were characterised using atomic force microscopy, X-ray photon spectroscopy, and optical and transmission electron microscopy. The contact angle does not influence the deposition of the layers. It was determined that it is possible to obtain nanometric oxide layers of a few micrometres in size. The chemical composition was determined by XPS and EDS independently, and showed that the oxide layer contains about 90 atom % of gallium with some additions of tin and zinc. The oxides obtained from the eutectic Ga–Sn–Zn liquid alloys appear to be nanocrystalline. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposiumc)
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16 pages, 5455 KiB  
Article
Tailoring Upconversion and Morphology of Yb/Eu Doped Y2O3 Nanostructures by Acid Composition Mediation
by Daniela Nunes, Ana Pimentel, Mariana Matias, Tomás Freire, A. Araújo, Filipe Silva, Patrícia Gaspar, Silvia Garcia, Patrícia A. Carvalho, Elvira Fortunato and Rodrigo Martins
Nanomaterials 2019, 9(2), 234; https://doi.org/10.3390/nano9020234 - 09 Feb 2019
Cited by 25 | Viewed by 4478
Abstract
The present study reports the production of upconverter nanostructures composed by a yttrium oxide host matrix co-doped with ytterbium and europium, i.e., Y2O3:Yb3+/Eu3+. These nanostructures were formed through the dissociation of yttrium, ytterbium and europium [...] Read more.
The present study reports the production of upconverter nanostructures composed by a yttrium oxide host matrix co-doped with ytterbium and europium, i.e., Y2O3:Yb3+/Eu3+. These nanostructures were formed through the dissociation of yttrium, ytterbium and europium oxides using acetic, hydrochloric and nitric acids, followed by a fast hydrothermal method assisted by microwave irradiation and subsequent calcination process. Structural characterization has been carried out by X-ray diffraction (XRD), scanning transmission electron microscopy (STEM) and scanning electron microscopy (SEM) both coupled with energy dispersive X-ray spectroscopy (EDS). The acid used for dissociation of the primary oxides played a crucial role on the morphology of the nanostructures. The acetic-based nanostructures resulted in nanosheets in the micrometer range, with thickness of around 50 nm, while hydrochloric and nitric resulted in sphere-shaped nanostructures. The produced nanostructures revealed a homogeneous distribution of the doping elements. The thermal behaviour of the materials has been investigated with in situ X-Ray diffraction and differential scanning calorimetry (DSC) experiments. Moreover, the optical band gaps of all materials were determined from diffuse reflectance spectroscopy, and their photoluminescence behaviour has been accessed showing significant differences depending on the acid used, which can directly influence their upconversion performance. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposiumc)
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9 pages, 1350 KiB  
Article
Fully Printed Zinc Oxide Electrolyte-Gated Transistors on Paper
by José Tiago Carvalho, Viorel Dubceac, Paul Grey, Inês Cunha, Elvira Fortunato, Rodrigo Martins, Andre Clausner, Ehrenfried Zschech and Luís Pereira
Nanomaterials 2019, 9(2), 169; https://doi.org/10.3390/nano9020169 - 30 Jan 2019
Cited by 32 | Viewed by 5560
Abstract
Fully printed and flexible inorganic electrolyte gated transistors (EGTs) on paper with a channel layer based on an interconnected zinc oxide (ZnO) nanoparticle matrix are reported in this work. The required rheological properties and good layer formation after printing are obtained using an [...] Read more.
Fully printed and flexible inorganic electrolyte gated transistors (EGTs) on paper with a channel layer based on an interconnected zinc oxide (ZnO) nanoparticle matrix are reported in this work. The required rheological properties and good layer formation after printing are obtained using an eco-friendly binder such as ethyl cellulose (EC) to disperse the ZnO nanoparticles. Fully printed devices on glass substrates using a composite solid polymer electrolyte as gate dielectric exhibit saturation mobility above 5 cm2 V−1 s−1 after annealing at 350 °C. Proper optimization of the nanoparticle content in the ink allows for the formation of a ZnO channel layer at a maximum annealing temperature of 150 °C, compatible with paper substrates. These devices show low operation voltages, with a subthreshold slope of 0.21 V dec−1, a turn on voltage of 1.90 V, a saturation mobility of 0.07 cm2 V−1 s−1 and an Ion/Ioff ratio of more than three orders of magnitude. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposiumc)
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18 pages, 9157 KiB  
Article
Growth Kinetics of the Selected Intermetallic Phases in Ni/Al/Ni System with Various Nickel Substrate Microstructure
by Izabella Kwiecien, Piotr Bobrowski, Anna Wierzbicka-Miernik, Lidia Litynska-Dobrzynska and Joanna Wojewoda-Budka
Nanomaterials 2019, 9(2), 134; https://doi.org/10.3390/nano9020134 - 22 Jan 2019
Cited by 15 | Viewed by 3557
Abstract
Reactivity in nickel–aluminum system was examined for two variants of nickel substrates in terms of the size and shape of Ni grains. The microstructure transformation aroused due to the annealing at 720 °C for different annealing times (0.25 to 72 h) was consequently [...] Read more.
Reactivity in nickel–aluminum system was examined for two variants of nickel substrates in terms of the size and shape of Ni grains. The microstructure transformation aroused due to the annealing at 720 °C for different annealing times (0.25 to 72 h) was consequently followed. The sequence of formation of the particular intermetallic phases was given. The interconnection zones were examined by means of scanning electron microscopy supported with energy dispersive X-ray spectroscopy and electron backscattered diffraction techniques as well as by the transmission electron microscopy. The growth kinetics data for AlNi, AlNiNi-rich and AlNi3 phases for both variants of substrates was given, indicating the differences obtained in previous works on this subject. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposiumc)
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16 pages, 9637 KiB  
Article
Effects of Residual Stress Distribution on Interfacial Adhesion of Magnetron Sputtered AlN and AlN/Al Nanostructured Coatings on a (100) Silicon Substrate
by Rashid Ali, Marco Renzelli, M. Imran Khan, Marco Sebastiani and Edoardo Bemporad
Nanomaterials 2018, 8(11), 896; https://doi.org/10.3390/nano8110896 - 01 Nov 2018
Cited by 19 | Viewed by 4165
Abstract
The present study investigated the influence of nanoscale residual stress depth gradients on the nano-mechanical behavior and adhesion energy of aluminium nitride (AlN) and Al/AlN sputtered thin films on a (100) silicon substrate. By using a focused ion beam (FIB) incremental ring-core method, [...] Read more.
The present study investigated the influence of nanoscale residual stress depth gradients on the nano-mechanical behavior and adhesion energy of aluminium nitride (AlN) and Al/AlN sputtered thin films on a (100) silicon substrate. By using a focused ion beam (FIB) incremental ring-core method, the residual stress depth gradient was assessed in the films in comparison with standard curvature residual stress measurements. The adhesion energy was then quantified by using a nanoindentation-based model. Results showed that the addition of an aluminum layer gave rise to additional tensile stress at the coating/substrate interface, which can be explained in terms of the differences of thermal expansion coefficients with the silicon substrate. Therefore, the coatings without the Al layer showed better adhesion because of a more homogeneous compressive residual stress in comparison with the coating having the Al layer, even though both groups of coatings were produced under the same bias voltage. Results are discussed, and some general suggestions are made on the correlation between coating/substrate property combinations and the adhesion energy of multilayer stacks. The results suggested that the Al bond layer and inhomogeneous residual stresses negatively affected the adhesion of AlN to a substrate such as silicon. Full article
(This article belongs to the Special Issue Characterization of Nanomaterials: Selected Papers from 6th Dresden Nanoanalysis Symposiumc)
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