Transmission Electron Microscopy for Nanomaterials Research Advances

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

Deadline for manuscript submissions: 30 November 2024 | Viewed by 9995

Special Issue Editors


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Guest Editor
Institute for Microelectronics and Microsystems, National Research Council, Via Monteroni, 73100 Lecce, Italy
Interests: transmission electron microscopy (TEM); scanning electron microscopy (SEM); focused ion beam (FIB); condensed matter physics; nanomaterials; radiation sensitive materials

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Guest Editor
Institute of Crystallography, National Research Council, Via Amendola 122/O, 70126 Bari, Italy
Interests: physics; electron microscopy; solid state physics; atomic resolution imaging and spectroscopies in TEM; electron diffraction; convergent beam electron diffraction (CBED); coherent electron diffraction imaging; in-line electron holography; low-dose atomic resolution imaging in TEM
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Special Issue Information

Dear Colleagues,

Since Ruska and Knoll proof of concept of transmission electron microscope, in 1931, technological advances and methodological development have made Transmission Electron Microscopy (TEM) a complex discipline, counting a vast variety of approaches to understand the morphological, structural, chemical and magnetic properties of the matter at the highest spatial resolution. Due to its strong transversality and high flexibility, TEM enables to solve fundamental and applied research problems, contributing to the progress in many fields of knowledge, such as physics, materials science, biology, medicine, engineering, chemistry, nanoscience and nanotechnology.

The last years have seen a further boost in TEM thanks to the introduction of effective aberration correctors for electron lenses, new detectors for imaging, diffraction and spectroscopies, monochromators on primary beam, new capabilities for in operando experiments, new tools for cryoEM, all complemented by the huge progress in computer science, pressing the development of novel methods to investigate organic and inorganic matter.

This special issue focuses on TEM studies for nanomaterials research advances. An upcoming aim is to show how the most recent technological and methodological developments in TEM impact on the comprehension of fundamental and subtle properties of nanomaterials, supplying the necessary knowledge for basic understanding of the nanoscience phenomena and for conscious design of new nanomaterials.

It is our pleasure to announce the opening of the submission for this special issue.

Full papers, communications, and reviews are all welcome.

Dr. Antonietta Taurino
Dr. Elvio Carlino
Guest Editors

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Keywords

  • HRTEM
  • HAADF
  • electron diffraction
  • 4DSTEM
  • electron holography
  • TEM tomography
  • EELS
  • EDS
  • in operando
  • cryoEM

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Published Papers (6 papers)

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Research

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14 pages, 7529 KiB  
Article
Direct Imaging of Radiation-Sensitive Organic Polymer-Based Nanocrystals at Sub-Ångström Resolution
by Elvio Carlino, Antonietta Taurino, Dritan Hasa, Dejan-Krešimir Bučar, Maurizio Polentarutti, Lidia E. Chinchilla and Josè J. Calvino Gamez
Nanomaterials 2024, 14(10), 872; https://doi.org/10.3390/nano14100872 - 17 May 2024
Viewed by 1465
Abstract
Seeing the atomic configuration of single organic nanoparticles at a sub-Å spatial resolution by transmission electron microscopy has been so far prevented by the high sensitivity of soft matter to radiation damage. This difficulty is related to the need to irradiate the particle [...] Read more.
Seeing the atomic configuration of single organic nanoparticles at a sub-Å spatial resolution by transmission electron microscopy has been so far prevented by the high sensitivity of soft matter to radiation damage. This difficulty is related to the need to irradiate the particle with a total dose of a few electrons/Å2, not compatible with the electron beam density necessary to search the low-contrast nanoparticle, to control its drift, finely adjust the electron-optical conditions and particle orientation, and finally acquire an effective atomic-resolution image. On the other hand, the capability to study individual pristine nanoparticles, such as proteins, active pharmaceutical ingredients, and polymers, with peculiar sensitivity to the variation in the local structure, defects, and strain, would provide advancements in many fields, including materials science, medicine, biology, and pharmacology. Here, we report the direct sub-ångström-resolution imaging at room temperature of pristine unstained crystalline polymer-based nanoparticles. This result is obtained by combining low-dose in-line electron holography and phase-contrast imaging on state-of-the-art equipment, providing an effective tool for the quantitative sub-ångström imaging of soft matter. Full article
(This article belongs to the Special Issue Transmission Electron Microscopy for Nanomaterials Research Advances)
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18 pages, 3359 KiB  
Article
Improved Method for Electron Powder Diffraction-Based Rietveld Analysis of Nanomaterials
by Viktória K. Kis, Zsolt Kovács and Zsolt Czigány
Nanomaterials 2024, 14(5), 444; https://doi.org/10.3390/nano14050444 - 28 Feb 2024
Cited by 1 | Viewed by 1099
Abstract
Multiphase nanomaterials are of increasing importance in material science. Providing reliable and statistically meaningful information on their average nanostructure is essential for synthesis control and applications. In this paper, we propose a novel procedure that simplifies and makes more effective the electron powder [...] Read more.
Multiphase nanomaterials are of increasing importance in material science. Providing reliable and statistically meaningful information on their average nanostructure is essential for synthesis control and applications. In this paper, we propose a novel procedure that simplifies and makes more effective the electron powder diffraction-based Rietveld analysis of nanomaterials. Our single step in-TEM method allows to obtain the instrumental broadening function of the TEM directly from a single measurement without the need for an additional X-ray diffraction measurement. Using a multilayer graphene calibration standard and applying properly controlled acquisition conditions on a spherical aberration-corrected microscope, we achieved the instrumental broadening of ±0.01 Å in terms of interplanar spacing. The shape of the diffraction peaks is modeled as a function of the scattering angle using the Caglioti relation, and the obtained parameters for instrumental broadening can be directly applied in the Rietveld analysis of electron diffraction data of the analyzed specimen. During peak shape analysis, the instrumental broadening parameters of the TEM are controlled separately from nanostructure-related peak broadening effects, which contribute to the higher reliability of nanostructure information extracted from electron diffraction patterns. The potential of the proposed procedure is demonstrated through the Rietveld analysis of hematite nanopowder and two-component Cu-Ni nanocrystalline thin film specimens. Full article
(This article belongs to the Special Issue Transmission Electron Microscopy for Nanomaterials Research Advances)
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15 pages, 11171 KiB  
Article
Unified Interpretations of Two Kinds of Needle-Shaped Precipitates Using Transmission Electron Microscopy and Small-Angle Neutron Scattering in Aged Al–Mg2Si(-Cu) Alloys
by Amalina Aina Kaharudin, Masato Ohnuma, Seungwon Lee, Taiki Tsuchiya, Yuuki Asada, Ken-ichi Ikeda, Kazuki Ohishi, Jun-ichi Suzuki, Kenji Matsuda and Tomoyuki Homma
Nanomaterials 2024, 14(2), 176; https://doi.org/10.3390/nano14020176 - 12 Jan 2024
Viewed by 1218
Abstract
This study investigates the nanostructural properties of pseudo-binary Al–1.0Mg2Si (mass%) alloys with and without 0.5Cu using transmission electron microscopy (TEM) and small-angle neutron scattering (SANS). The TEM results show that both alloys exhibit extra electron diffraction spots related to MgSiMg second [...] Read more.
This study investigates the nanostructural properties of pseudo-binary Al–1.0Mg2Si (mass%) alloys with and without 0.5Cu using transmission electron microscopy (TEM) and small-angle neutron scattering (SANS). The TEM results show that both alloys exhibit extra electron diffraction spots related to MgSiMg second clusters at peak-aged conditions. High-resolution TEM images have revealed that the second cluster exists as a needle-shaped precipitate that is shorter and thicker than the β″ phase. We found that the second cluster, which we referred to as the R phase in this paper, is more likely to form partially along the longitudinal axis of a random-type precipitate. Thus, the atomic arrangement in the random-type precipitate is not completely random. SANS is used to quantify the size and volume fraction of the observed needle-shaped precipitates since the R phase is difficult to observe with TEM. The R phase forms even in the Cu-free alloy, but the volume fraction is low, and the growth and formation are retarded near the peak-aged conditions. Undoubtedly, the Cu addition has the effect of stabilizing the growth of the R phase and also promoting its formation. Therefore, the R phase also contributes to the increase in hardness at both under- and peak-aged conditions in the Cu-containing alloy in addition to the strengthening β″ phases. Full article
(This article belongs to the Special Issue Transmission Electron Microscopy for Nanomaterials Research Advances)
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17 pages, 9643 KiB  
Article
Simple ePDF: A Pair Distribution Function Method Based on Electron Diffraction Patterns to Reveal the Local Structure of Amorphous and Nanocrystalline Materials
by János L. Lábár, Klára Hajagos-Nagy, Partha P. Das, Alejandro Gomez-Perez and György Radnóczi
Nanomaterials 2023, 13(24), 3136; https://doi.org/10.3390/nano13243136 - 14 Dec 2023
Cited by 1 | Viewed by 2306
Abstract
Amorphous, glassy or disordered materials play important roles in developing structural materials from metals or ceramics, devices from semiconductors or medicines from organic compounds. Their local structure is frequently similar to crystalline ones. A computer program is presented here that runs under the [...] Read more.
Amorphous, glassy or disordered materials play important roles in developing structural materials from metals or ceramics, devices from semiconductors or medicines from organic compounds. Their local structure is frequently similar to crystalline ones. A computer program is presented here that runs under the Windows operating system on a PC to extract pair distribution function (PDF) from electron diffraction in a transmission electron microscope (TEM). A polynomial correction reduces small systematic deviations from the expected average Q-dependence of scattering. Neighbor distance and coordination number measurements are supplemented by either measurement or enforcement of number density. Quantification of similarity is supported by calculation of Pearson’s correlation coefficient and fingerprinting. A rough estimate of fractions in a mixture is computed by multiple least-square fitting using the PDFs from components of the mixture. PDF is also simulated from crystalline structural models (in addition to measured ones) to be used in libraries for fingerprinting or fraction estimation. Crystalline structure models for simulations are obtained from CIF files or str files of ProcessDiffraction. Data from inorganic samples exemplify usage. In contrast to previous free ePDF programs, our stand-alone program does not need a special software environment, which is a novelty. The program is available from the author upon request. Full article
(This article belongs to the Special Issue Transmission Electron Microscopy for Nanomaterials Research Advances)
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10 pages, 3407 KiB  
Article
The Atomic Observation of the Structural Change Process in Pt Networks in Air Using Environmental Cell Scanning Transmission Electron Microscopy
by Masaki Takeguchi, Toshiaki Takei and Kazutaka Mitsuishi
Nanomaterials 2023, 13(15), 2170; https://doi.org/10.3390/nano13152170 - 26 Jul 2023
Cited by 2 | Viewed by 1096
Abstract
The structural change in Pt networks composed of multiple chain connections among grains was observed in air at 1 atm using atomic-resolution environmental cell scanning transmission electron microscopy. An aberration-corrected incident electron probe with a wide convergence angle made it possible to increase [...] Read more.
The structural change in Pt networks composed of multiple chain connections among grains was observed in air at 1 atm using atomic-resolution environmental cell scanning transmission electron microscopy. An aberration-corrected incident electron probe with a wide convergence angle made it possible to increase the depth resolution that contributes to enhancing the signal-to-noise ratio of Pt network samples in air in an environmental cell, resulting in the achievement of atomic-resolution imaging. The exposure of the Pt networks to gas molecules under Brownian motion, stimulated by electron beams in the air, increases the collision probability between gas molecules and Pt networks, and the Pt networks are more intensely stressed from all directions than in a situation without electron irradiation. By increasing the electron beam dose rate, the structural change of the Pt networks became significant. Dynamic observation on an atomic scale suggested that the structural change of the networks was not attributed to the surface atomic-diffusion-induced step motion but mainly caused by the movement and deformation of unstable grains and grain boundaries. The oxidized surface layers may be one of the factors hindering the surface atomic step motion, mitigating the change in the size of the grains and grain boundaries. Full article
(This article belongs to the Special Issue Transmission Electron Microscopy for Nanomaterials Research Advances)
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Review

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7 pages, 2426 KiB  
Review
Role of Interdiffusion and Segregation during the Life of Indium Gallium Arsenide Quantum Dots, from Cradle to Grave
by Thomas Walther
Nanomaterials 2022, 12(21), 3850; https://doi.org/10.3390/nano12213850 - 31 Oct 2022
Cited by 3 | Viewed by 1441
Abstract
This article summarizes our understanding of the interplay between diffusion and segregation during epitaxial growth of InGaAs and InAs quantum dots. These quantum dots form spontaneously on flat GaAs (001) single-crystalline substrates by the so-called Stranski-Krastanow growth mechanism once a sufficient amount of [...] Read more.
This article summarizes our understanding of the interplay between diffusion and segregation during epitaxial growth of InGaAs and InAs quantum dots. These quantum dots form spontaneously on flat GaAs (001) single-crystalline substrates by the so-called Stranski-Krastanow growth mechanism once a sufficient amount of indium has accumulated on the surface. Initially a perfectly flat wetting layer is formed. This strained layer then starts to roughen as strain increases, leading first to small, long-range surface undulations and then to tiny coherent islands. These continue to grow, accumulating indium both from the underlying wetting layer by lateral indium segregation and from within these islands by vertical segregation, which for InGaAs deposition results in an indium-enriched InGaAs alloy in the centre of the quantum dots. For pure InAs deposition, interdiffusion also results in an InGaAs alloy. Further deposition can lead to the formation of misfit dislocations that nucleate at the edges of the islands and are generally sought to be avoided. Overgrowth by GaAs or InGaAs alloys with low indium content commences preferentially between the islands, avoiding their strained edges, which initially leads to trench formation. Further deposition is necessary to cap these quantum dots effectively and to re-gain an almost flat surface that can then be used for subsequent deposition of multiple layers of quantum dots as needed for many optoelectronic devices. Full article
(This article belongs to the Special Issue Transmission Electron Microscopy for Nanomaterials Research Advances)
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