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Materials Characterizations Using In-Situ Techniques
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Materials Characterizations Using In-Situ Techniques

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

Deadline for manuscript submissions: closed (10 May 2022) | Viewed by 27224

Special Issue Editors

Dr. Zibin Chen

E-Mail Website
Guest Editor
School of Aerospace, Mechanical and Mechatronic Engineering, the University of Sydney, Sydney, NSW 2006, Australia
Interests: electron microscopy; multiferroic materials; quantum dots; metals and alloys; ceramics
Prof. Dr. Xiaozhou Liao

E-Mail Website
Guest Editor
School of Aerospace, Mechanical and Mechatronic Engineering, the University of Sydney, Sydney, NSW 2006, Australia
Interests: electron microscopy; synthesis/processing–structure–property relationship; nanomaterials; metals and alloys; ceramics; ferroelectrics
Prof. Dr. Wenge Yang

E-Mail Website
Guest Editor
Center for High Pressure Science and Technology Advanced Research, 1690 Cailun Road, Shanghai, China
Interests: high pressure science; structure phase transition; geophysics; synchrotron radiation; extreme conditions

Special Issue Information

Dear Colleagues,

It is well-known that the properties of materials are closely related to their microstructures. Understanding the structure–property relationships of materials is therefore critical for designing materials with superior properties that meet the application requirements. Most previous studies of the structure–property relationships of materials were mainly carried out through separate property measurement and structural characterization, which in many cases do not reveal the real nature of materials’ behaviour under external stimuli (e.g., force, heat, and voltage) and the fundamental origins of materials’ properties. With the development of material characterization technology, it is now possible to conduct simultaneous in situ mechanical and physical property measurements and structural characterization using methods including optical microscopy, electron microscopy, X-ray diffraction, and scanning probe microscopy. The development of state-of-the-art in situ characterization techniques has significantly advanced our understanding of the structure–property relationships of materials. Here, we propose a Special Issue in Materials focusing on recent advances in in situ microscopy techniques and their applications in materials research. Contributions in the forms of review articles and research papers are all welcome. Content covered in this Special Issue will include but is not limited to the following fields:

  • In situ structural characterization using optical microscopy, electron microscopy, scanning probe microscopy, and synchrotron radiation techniques;
  • In situ property measurement/testing;
  • Development of in situ techniques;
  • Dynamic simulations to uncover deformation mechanisms and/or fundamental physics of materials.

Dr. Zibin Chen
Prof. Dr. Xiaozhou Liao
Prof. Dr. Wenge Yang
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. 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

  • in situ
  • simulation
  • characterization
  • electron microscopy
  • synchrotron radiation
  • optical microscopy
  • scanning probe microscopy

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Related Special Issue

Published Papers (8 papers)

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Research

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12 pages, 5754 KiB  
Article
Investigating Iron Alloy Phase Changes Using High Temperature In Situ SEM Techniques
by Rhiannon Heard, Clive R. Siviour and Kalin Dragnevski
Materials 2022, 15(11), 3921; https://doi.org/10.3390/ma15113921 - 31 May 2022
Cited by 1 | Viewed by 1714
Abstract
This research utilises a novel heat stage combined with a Zeiss scanning electron microscope to investigate phase changes in iron alloys at temperatures up to 800 ℃ using SE and EBSD imaging. Carbon steel samples with starting structures of ferrite/pearlite were transformed into [...] Read more.
This research utilises a novel heat stage combined with a Zeiss scanning electron microscope to investigate phase changes in iron alloys at temperatures up to 800 ℃ using SE and EBSD imaging. Carbon steel samples with starting structures of ferrite/pearlite were transformed into austenite using the commercial heat treatment process whilst imaging within the SEM. This process facilitates capturing both grain and phase transformation in real time allowing better insight into the microstructural evolution and overall phase change kinetics of this heat treatment. The technique for imaging uses a combination of localised EBSD high temperature imaging combined with the development of high temperature thermal-etching SE imaging technique. The SE thermal etching technique, as verified by EBSD images, enables tracking of a statistically significant number of grains (>100) and identification of individual phases. As well as being applied to carbon steel as shown here, the technique is part of a larger study on high temperature in situ SEM techniques and could be applied to a variety of alloys to study complex phase transformations. Full article
(This article belongs to the Special Issue Materials Characterizations Using In-Situ Techniques)
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12 pages, 55655 KiB  
Article
Environmental STEM Study of the Oxidation Mechanism for Iron and Iron Carbide Nanoparticles
by Alec P. LaGrow, Simone Famiani, Andreas Sergides, Leonardo Lari, David C. Lloyd, Mari Takahashi, Shinya Maenosono, Edward D. Boyes, Pratibha L. Gai and Nguyen Thi Kim Thanh
Materials 2022, 15(4), 1557; https://doi.org/10.3390/ma15041557 - 18 Feb 2022
Cited by 5 | Viewed by 2396
Abstract
The oxidation of solution-synthesized iron (Fe) and iron carbide (Fe2C) nanoparticles was studied in an environmental scanning transmission electron microscope (ESTEM) at elevated temperatures under oxygen gas. The nanoparticles studied had a native oxide shell present, that formed after synthesis, an [...] Read more.
The oxidation of solution-synthesized iron (Fe) and iron carbide (Fe2C) nanoparticles was studied in an environmental scanning transmission electron microscope (ESTEM) at elevated temperatures under oxygen gas. The nanoparticles studied had a native oxide shell present, that formed after synthesis, an ~3 nm iron oxide (FexOy) shell for the Fe nanoparticles and ~2 nm for the Fe2C nanoparticles, with small void areas seen in several places between the core and shell for the Fe and an ~0.8 nm space between the core and shell for the Fe2C. The iron nanoparticles oxidized asymmetrically, with voids on the borders between the Fe core and FexOy shell increasing in size until the void coalesced, and finally the Fe core disappeared. In comparison, the oxidation of the Fe2C progressed symmetrically, with the core shrinking in the center and the outer oxide shell growing until the iron carbide had fully disappeared. Small bridges of iron oxide formed during oxidation, indicating that the Fe transitioned to the oxide shell surface across the channels, while leaving the carbon behind in the hollow core. The carbon in the carbide is hypothesized to suppress the formation of larger crystallites of iron oxide during oxidation, and alter the diffusion rates of the Fe and O during the reaction, which explains the lower sensitivity to oxidation of the Fe2C nanoparticles. Full article
(This article belongs to the Special Issue Materials Characterizations Using In-Situ Techniques)
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10 pages, 1867 KiB  
Article
In Situ Observation of Liquid Solder Alloys and Solid Substrate Reactions Using High-Voltage Transmission Electron Microscopy
by Xin F. Tan, Flora Somidin, Stuart D. McDonald, Michael J. Bermingham, Hiroshi Maeno, Syo Matsumura and Kazuhiro Nogita
Materials 2022, 15(2), 510; https://doi.org/10.3390/ma15020510 - 10 Jan 2022
Cited by 4 | Viewed by 2234
Abstract
The complex reaction between liquid solder alloys and solid substrates has been studied ex-situ in a few studies, utilizing creative setups to “freeze” the reactions at different stages during the reflow soldering process. However, full understanding of the dynamics of the process is [...] Read more.
The complex reaction between liquid solder alloys and solid substrates has been studied ex-situ in a few studies, utilizing creative setups to “freeze” the reactions at different stages during the reflow soldering process. However, full understanding of the dynamics of the process is difficult due to the lack of direct observation at micro- and nano-meter resolutions. In this study, high voltage transmission electron microscopy (HV-TEM) is employed to observe the morphological changes that occur in Cu6Sn5 between a Sn-3.0 wt%Ag-0.5 wt%Cu (SAC305) solder alloy and a Cu substrate in situ at temperatures above the solidus of the alloy. This enables the continuous surveillance of rapid grain boundary movements of Cu6Sn5 during soldering and increases the fundamental understanding of reaction mechanisms in solder solid/liquid interfaces. Full article
(This article belongs to the Special Issue Materials Characterizations Using In-Situ Techniques)
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10 pages, 3685 KiB  
Article
Investigation of Deoxidation Process of MoO3 Using Environmental TEM
by Peijie Ma, Ang Li, Lihua Wang and Kun Zheng
Materials 2022, 15(1), 56; https://doi.org/10.3390/ma15010056 - 22 Dec 2021
Cited by 4 | Viewed by 3365
Abstract
In situ environmental transmission electron microscope (ETEM) could provide intuitive and solid proof for the local structure and chemical evolution of materials under practical working conditions. In particular, coupled with atmosphere and thermal field, the behavior of nano catalysts could be directly observed [...] Read more.
In situ environmental transmission electron microscope (ETEM) could provide intuitive and solid proof for the local structure and chemical evolution of materials under practical working conditions. In particular, coupled with atmosphere and thermal field, the behavior of nano catalysts could be directly observed during the catalytic reaction. Through the change of lattice structure, it can directly correlate the relationship between the structure, size and properties of materials in the nanoscale, and further directly and accurately, which is of great guiding value for the study of catalysis mechanism and the optimization of catalysts. As an outstanding catalytic material in the application of methane reforming, molybdenum oxide (MoO3)-based materials and its deoxidation process were studied by in situ ETEM method. The corresponding microstructures and components evolution were analyzed by diffraction, high-resolution transmission electron microscopy (HRTEM) and electron energy loss spectrum (EELS) techniques. MoO3 had a good directional deoxidation process accompanied with the process of nanoparticles crushing and regrowth in hydrogen (H2) and thermal field. However, in the absence of H2, the samples would exhibit different structural evolution. Full article
(This article belongs to the Special Issue Materials Characterizations Using In-Situ Techniques)
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13 pages, 2975 KiB  
Article
Monitoring Electrical Biasing of Pb(Zr0.2Ti0.8)O3 Ferroelectric Thin Films In Situ by DPC-STEM Imaging
by Alexander Vogel, Martin F. Sarott, Marco Campanini, Morgan Trassin and Marta D. Rossell
Materials 2021, 14(16), 4749; https://doi.org/10.3390/ma14164749 - 23 Aug 2021
Cited by 5 | Viewed by 3844
Abstract
Increased data storage densities are required for the next generation of nonvolatile random access memories and data storage devices based on ferroelectric materials. Yet, with intensified miniaturization, these devices face a loss of their ferroelectric properties. Therefore, a full microscopic understanding of the [...] Read more.
Increased data storage densities are required for the next generation of nonvolatile random access memories and data storage devices based on ferroelectric materials. Yet, with intensified miniaturization, these devices face a loss of their ferroelectric properties. Therefore, a full microscopic understanding of the impact of the nanoscale defects on the ferroelectric switching dynamics is crucial. However, collecting real-time data at the atomic and nanoscale remains very challenging. In this work, we explore the ferroelectric response of a Pb(Zr0.2Ti0.8)O3 thin film ferroelectric capacitor to electrical biasing in situ in the transmission electron microscope. Using a combination of high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and differential phase contrast (DPC)-STEM imaging we unveil the structural and polarization state of the ferroelectric thin film, integrated into a capacitor architecture, before and during biasing. Thus, we can correlate real-time changes in the DPC signal with the presence of misfit dislocations and ferroelastic domains. A reduction in the domain wall velocity of 24% is measured in defective regions of the film when compared to predominantly defect-free regions. Full article
(This article belongs to the Special Issue Materials Characterizations Using In-Situ Techniques)
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13 pages, 5055 KiB  
Article
Machine Learning Assisted Classification of Aluminum Nitride Thin Film Stress via In-Situ Optical Emission Spectroscopy Data
by Yu-Pu Yang, Te-Yun Lu, Hsiao-Han Lo, Wei-Lun Chen, Peter J. Wang, Walter Lai, Yiin-Kuen Fuh and Tomi T. Li
Materials 2021, 14(16), 4445; https://doi.org/10.3390/ma14164445 - 8 Aug 2021
Cited by 8 | Viewed by 3379
Abstract
In this study, we submit a complex set of in-situ data collected by optical emission spectroscopy (OES) during the process of aluminum nitride (AlN) thin film. Changing the sputtering power and nitrogen(N2) flow rate, AlN film was deposited on Si substrate [...] Read more.
In this study, we submit a complex set of in-situ data collected by optical emission spectroscopy (OES) during the process of aluminum nitride (AlN) thin film. Changing the sputtering power and nitrogen(N2) flow rate, AlN film was deposited on Si substrate using a superior sputtering with a pulsed direct current (DC) method. The correlation between OES data and deposited film residual stress (tensile vs. compressive) associated with crystalline status by X-ray diffraction spectroscopy (XRD), scanning electron microscope (SEM), and transmission electron microscope (TEM) measurements were investigated and established throughout the machine learning exercise. An important answer to know is whether the stress of the processing film is compressive or tensile. To answer this question, we can access as many optical spectra data as we need, record the data to generate a library, and exploit principal component analysis (PCA) to reduce complexity from complex data. After preprocessing through PCA, we demonstrated that we could apply standard artificial neural networks (ANNs), and we could obtain a machine learning classification method to distinguish the stress types of the AlN thin films obtained by analyzing XRD results and correlating with TEM microstructures. Combining PCA with ANNs, an accurate method for in-situ stress prediction and classification was created to solve the semiconductor process problems related to film property on deposited films more efficiently. Therefore, methods for machine learning-assisted classification can be further extended and applied to other semiconductors or related research of interest in the future. Full article
(This article belongs to the Special Issue Materials Characterizations Using In-Situ Techniques)
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Review

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27 pages, 30501 KiB  
Review
X-ray Imaging of Alloy Solidification: Crystal Formation, Growth, Instability and Defects
by Shikang Feng, Enzo Liotti and Patrick S. Grant
Materials 2022, 15(4), 1319; https://doi.org/10.3390/ma15041319 - 10 Feb 2022
Cited by 10 | Viewed by 3341
Abstract
Synchrotron and laboratory-based X-ray imaging techniques have been increasingly used for in situ investigations of alloy solidification and other metal processes. Several reviews have been published in recent years that have focused on the development of in situ X-ray imaging techniques for metal [...] Read more.
Synchrotron and laboratory-based X-ray imaging techniques have been increasingly used for in situ investigations of alloy solidification and other metal processes. Several reviews have been published in recent years that have focused on the development of in situ X-ray imaging techniques for metal solidification studies. Instead, this work provides a comprehensive review of knowledge provided by in situ X-ray imaging for improved understanding of solidification theories and emerging metal processing technologies. We first review insights related to crystal nucleation and growth mechanisms gained by in situ X-ray imaging, including solute suppressed nucleation theory of α-Al and intermetallic compound crystals, dendritic growth of α-Al and the twin plane re-entrant growth mechanism of faceted Fe-rich intermetallics. Second, we discuss the contribution of in situ X-ray studies in understanding microstructural instability, including dendrite fragmentation induced by solute-driven, dendrite root re-melting, instability of a planar solid/liquid interface, the cellular-to-dendritic transition and the columnar-to-equiaxed transition. Third, we review investigations of defect formation mechanisms during near-equilibrium solidification, including porosity and hot tear formation, and the associated liquid metal flow. Then, we discuss how X-ray imaging is being applied to the understanding and development of emerging metal processes that operate further from equilibrium, such as additive manufacturing. Finally, the outlook for future research opportunities and challenges is presented. Full article
(This article belongs to the Special Issue Materials Characterizations Using In-Situ Techniques)
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20 pages, 5306 KiB  
Review
Structural Phase Transition and In-Situ Energy Storage Pathway in Nonpolar Materials: A Review
by Xian-Kui Wei, Rafal E. Dunin-Borkowski and Joachim Mayer
Materials 2021, 14(24), 7854; https://doi.org/10.3390/ma14247854 - 18 Dec 2021
Cited by 18 | Viewed by 4905
Abstract
Benefitting from exceptional energy storage performance, dielectric-based capacitors are playing increasingly important roles in advanced electronics and high-power electrical systems. Nevertheless, a series of unresolved structural puzzles represent obstacles to further improving the energy storage performance. Compared with ferroelectrics and linear dielectrics, antiferroelectric [...] Read more.
Benefitting from exceptional energy storage performance, dielectric-based capacitors are playing increasingly important roles in advanced electronics and high-power electrical systems. Nevertheless, a series of unresolved structural puzzles represent obstacles to further improving the energy storage performance. Compared with ferroelectrics and linear dielectrics, antiferroelectric materials have unique advantages in unlocking these puzzles due to the inherent coupling of structural transitions with the energy storage process. In this review, we summarize the most recent studies about in-situ structural phase transitions in PbZrO3-based and NaNbO3-based systems. In the context of the ultrahigh energy storage density of SrTiO3-based capacitors, we highlight the necessity of extending the concept of antiferroelectric-to-ferroelectric (AFE-to-FE) transition to broader antiferrodistortive-to-ferrodistortive (AFD-to-FD) transition for materials that are simultaneously ferroelastic. Combining discussion of the factors driving ferroelectricity, electric-field-driven metal-to-insulator transition in a (La1−xSrx)MnO3 electrode is emphasized to determine the role of ionic migration in improving the storage performance. We believe that this review, aiming at depicting a clearer structure–property relationship, will be of benefit for researchers who wish to carry out cutting-edge structure and energy storage exploration. Full article
(This article belongs to the Special Issue Materials Characterizations Using In-Situ Techniques)
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