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Microscopy in Material Science: Imaging, Analytics, and New Materials

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A special issue of Materials (ISSN 1996-1944). This special issue belongs to the section "Advanced Materials Characterization".

Deadline for manuscript submissions: closed (20 November 2022) | Viewed by 15042

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Special Issue Editor

Dr. Nabila Maloufi

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Guest Editor

1. LEM3, Université de Lorraine, CNRS, 57070 Metz, France
2. Labex Damas, Université de Lorraine, 57073 Metz, France
Interests: physical properties of materials; electron microscopy; development of innovative procedures in SEM; modeling; metallurgy; semiconductors

Special Issue Information

Dear Colleagues,

Microscopy techniques have become essential in the field of academic or private research, ranging from life science to nanotechnology or fundamental physics as well as for quality control in various industries.

Numerous material properties are probed in these well-known microscopes, which are otherwise complementary: light microscope, transmission electron microscope (TEM and high-resolution TEM, scanning TEM), and scanning electron microscope (SEM). These versatile, high-performance tools enable access, with their own corresponding resolutions, to many material properties, such as structure, morphology, texture, microstructure, and chemical composition, and the identification of defects, mechanical behavior using in situ tensile testing inside a SEM or a TEM, and drift or charge carrier diffusion information in semiconductors, fluorescence, etc.

The evolution and optimization over the past few years of the microscopy-associated techniques for characterizing a wide range of materials at different scales, from the bulk to the atomic level, has allowed huge progress in the understanding of links between their features. The following list of methods is not exhaustive: convergent beam electron diffraction, electron energy loss spectroscopy, three-dimensional electron back-scatter diffraction, accurate electron channeling contrast imaging, transmission Kikuchi diffraction, chemical reaction using liquid-phase electron microscopy, electron-beam-induced current, time-resolved cathodoluminescence, correlative light and electron microscopy methods, digital image correlation approaches, etc. Furthermore, these techniques play an important role in the enhancement and development of new materials and more sophisticated structures.

This Special Issue is devoted to innovative microscopy procedures, either to improve resolution and detection limits or to probe new properties. The implementation of methods combining in situ microscopy characterizations and physical or chemical analyses is also encouraged. The topics of interest also include the processing of microscopy data by advanced digital techniques as well as simulations and modeling. Furthermore, the latest research studies where microscopy has played an important role are welcomed, such as in the development of new materials or advanced systems, in the improvement of their properties, or in the discovery of new properties.

Dr. Nabila Maloufi
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. Materials 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 2600 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

new procedures in microscopy
SEM
TEM
modeling and simulations in microscopy
in situ microscopy techniques
new materials or complex systems and microscopy
materials properties and microscopy

Published Papers (5 papers)

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Research

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22 pages, 6368 KiB

Open AccessArticle

High Resolution Powder Electron Diffraction in Scanning Electron Microscopy

by Miroslav Slouf, Radim Skoupy, Ewa Pavlova and Vladislav Krzyzanek

Materials 2021, 14(24), 7550; https://doi.org/10.3390/ma14247550 - 9 Dec 2021

Cited by 5 | Viewed by 3633

Abstract

A modern scanning electron microscope equipped with a pixelated detector of transmitted electrons can record a four-dimensional (4D) dataset containing a two-dimensional (2D) array of 2D nanobeam electron diffraction patterns; this is known as a four-dimensional scanning transmission electron microscopy (4D-STEM). In this work, we introduce a new version of our method called 4D-STEM/PNBD (powder nanobeam diffraction), which yields high-resolution powder diffractograms, whose quality is fully comparable to standard TEM/SAED (selected-area electron diffraction) patterns. Our method converts a complex 4D-STEM dataset measured on a nanocrystalline material to a single 2D powder electron diffractogram, which is easy to process with standard software. The original version of 4D-STEM/PNBD method, which suffered from low resolution, was improved in three important areas: (i) an optimized data collection protocol enables the experimental determination of the point spread function (PSF) of the primary electron beam, (ii) an improved data processing combines an entropy-based filtering of the whole dataset with a PSF-deconvolution of the individual 2D diffractograms and (iii) completely re-written software automates all calculations and requires just a minimal user input. The new method was applied to Au, TbF₃ and TiO₂ nanocrystals and the resolution of the 4D-STEM/PNBD diffractograms was even slightly better than that of TEM/SAED. Full article

(This article belongs to the Special Issue Microscopy in Material Science: Imaging, Analytics, and New Materials)

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13 pages, 3625 KiB

Open AccessArticle

The Design of a Reflection Electron Energy Loss Spectrometer Attachment for Low Voltage Scanning Electron Microscopy

by Jonathan Chuah and Anjam Khursheed

Materials 2021, 14(24), 7511; https://doi.org/10.3390/ma14247511 - 7 Dec 2021

Viewed by 2199

Abstract

This paper presents the design of a reflection electron energy spectrometer (REELS) attachment for low voltage scanning electron microscopy (LVSEM) applications. The design is made by carrying out a scattered electron trajectory ray paths simulation. The spectrometer attachment is small enough to fit on the specimen stage of an SEM, and aims to acquire nanoscale spatially resolved REELS information. It uses a retarding field electrostatic toroidal sector energy analyzer design, which is able to lower the kinetic energies of elastically backscattered electrons to pass energies of 10 eV or less. For the capture of 1 keV BSEs emitted in the polar angular range between 40 to 50°, direct ray-tracing simulations predict that the spectrometer attachment will have an energy resolution of around 0.4 eV at a pass energy of 10 eV, and 0.2 eV at a pass energy of 5 eV. This predicted performance will make it a suitable REELS attachment for SEMs that use field emission electron sources. Full article

(This article belongs to the Special Issue Microscopy in Material Science: Imaging, Analytics, and New Materials)

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10 pages, 2299 KiB

Open AccessArticle

Modelling Electron Channeling Contrast Intensity of Stacking Fault and Twin Boundary Using Crystal Thickness Effect

by Hana Kriaa, Antoine Guitton and Nabila Maloufi

Materials 2021, 14(7), 1696; https://doi.org/10.3390/ma14071696 - 30 Mar 2021

Cited by 7 | Viewed by 1794

Abstract

In a scanning electron microscope, the backscattered electron intensity modulations are at the origin of the contrast of like-Kikuchi bands and crystalline defects. The Electron Channeling Contrast Imaging (ECCI) technique is suited for defects characterization at a mesoscale with transmission electron microscopy-like resolution. In order to achieve a better comprehension of ECCI contrasts of twin-boundary and stacking fault, an original theoretical approach based on the dynamical diffraction theory is used. The calculated backscattered electron intensity is explicitly expressed as function of physical and practical parameters controlling the ECCI experiment. Our model allows, first, the study of the specimen thickness effect on the channeling contrast on a perfect crystal, and thus its effect on the formation of like-Kikuchi bands. Then, our theoretical approach is extended to an imperfect crystal containing a planar defect such as twin-boundary and stacking fault, clarifying the intensity oscillations observed in ECC micrographs. Full article

(This article belongs to the Special Issue Microscopy in Material Science: Imaging, Analytics, and New Materials)

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12 pages, 5385 KiB

Open AccessEditor’s ChoiceArticle

Four-Fold Multi-Modal X-ray Microscopy Measurements of a Cu(In,Ga)Se₂ Solar Cell

by Christina Ossig, Christian Strelow, Jan Flügge, Andreas Kolditz, Jan Siebels, Jan Garrevoet, Kathryn Spiers, Martin Seyrich, Dennis Brückner, Niklas Pyrlik, Johannes Hagemann, Frank Seiboth, Andreas Schropp, Romain Carron, Gerald Falkenberg, Alf Mews, Christian G. Schroer, Tobias Kipp and Michael E. Stuckelberger

Materials 2021, 14(1), 228; https://doi.org/10.3390/ma14010228 - 5 Jan 2021

Cited by 12 | Viewed by 3208

Abstract

Inhomogeneities and defects often limit the overall performance of thin-film solar cells. Therefore, sophisticated microscopy approaches are sought to characterize performance and defects at the nanoscale. Here, we demonstrate, for the first time, the simultaneous assessment of composition, structure, and performance in four-fold [...] Read more.

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(CIGS) solar cell, we measured the elemental distribution of the key absorber elements, the electrical and optical response, and the phase shift of the coherent X-rays with nanoscale resolution. We found structural features in the absorber layer—interpreted as voids—that correlate with poor electrical performance and point towards defects that limit the overall solar cell efficiency. Full article

(This article belongs to the Special Issue Microscopy in Material Science: Imaging, Analytics, and New Materials)

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Review

Jump to: Research

22 pages, 5530 KiB

Open AccessReview

Zirconolite Polytypes and Murataite Polysomes in Matrices for the REE—Actinide Fraction of HLW

by Sergey V. Yudintsev, Maximilian S. Nickolsky, Michael I. Ojovan, Olga I. Stefanovsky, Boris S. Nikonov and Amina S. Ulanova

Materials 2022, 15(17), 6091; https://doi.org/10.3390/ma15176091 - 2 Sep 2022

Cited by 10 | Viewed by 1499

Abstract

Electron backscatter diffraction (EBSD) has been used for more than 30 years for analyzing the structure of minerals and artificial substances. In recent times, EBSD has been widely applied for investigation of irradiated nuclear fuel and matrices for the immobilization of radioactive waste. The combination of EBSD and scanning electron microscopy (SEM/EDS) methods allows researchers to obtain simultaneously data on a specimen’s local composition and structure. The article discusses the abilities of SEM/EDS and EBSD techniques to identify zirconolite polytype modifications and members of the polysomatic murataite–pyrochlore series in polyphase ceramic matrices, with simulations of Pu (Th) and the REE-actinide fraction (Nd) of high-level radioactive waste. Full article

(This article belongs to the Special Issue Microscopy in Material Science: Imaging, Analytics, and New Materials)

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