Scanning Electron Microscopy and Energy-Dispersive Spectroscopy Analyses in Materials Science

A special issue of Applied Sciences (ISSN 2076-3417). This special issue belongs to the section "Materials Science and Engineering".

Deadline for manuscript submissions: 31 May 2024 | Viewed by 8570

Special Issue Editors

Faculty of Materials Science and Engineering, “Gheorghe Asachi” Technical University of Iasi, 700050 Iasi, Romania
Interests: SEM; EDS; EBSD; AFM; biomaterials; biodegradable; ceramic layers; 3D printing
Special Issues, Collections and Topics in MDPI journals
Department of Materials Science, “Gheorghe Asachi” Technical University of Iasi, 700050 Iasi, Romania
Interests: corrosion resistance; electro-corrosion; EIS; polymers

Special Issue Information

Dear Colleagues,

Microstructure and chemical composition of metallic and non-metallic materials play a decisive role in materials’ properties. Obtaining extraordinary characteristics of materials can be achieved primarily by changing their structure and chemical composition. Each alloy system can be considered a small universe with unique properties and infinite possible modifications of properties from the atomic to the macro scale. Alloying and modifying surface properties can fundamentally change the characteristics of a material. Electron and atomic force microscopy along with chemical composition determinations from the nano to the millimeter scale provide precious information about the actual state of the material and lead to opportunities to improve their properties.

Prof. Dr. Nicanor Cimpoesu
Dr. Ramona Cimpoesu
Guest Editors

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Keywords

  • SEM
  • EDS
  • EBSD
  • WDX
  • AFM
  • nano/micro-FTIR
  • material science

Published Papers (6 papers)

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Research

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14 pages, 12744 KiB  
Article
Study on the Thermal Fatigue Effect of Carboxymethylcellulose Solution Media Dissolved in Water as a Quenching Cooling Medium
Appl. Sci. 2023, 13(10), 6021; https://doi.org/10.3390/app13106021 - 14 May 2023
Cited by 2 | Viewed by 993
Abstract
The degradation of a quenching cooling medium is a particularly important technical aspect in the technology of primary and final thermal treatments. This paper studied the effect of the thermal cycles of heating and cooling on a tempering medium type of 2.5% carboxymethyl [...] Read more.
The degradation of a quenching cooling medium is a particularly important technical aspect in the technology of primary and final thermal treatments. This paper studied the effect of the thermal cycles of heating and cooling on a tempering medium type of 2.5% carboxymethyl cellulose solution in water. The main characteristic of a cooling medium is the absorption of heat from the part, which is influenced by the physico-chemical characteristics of the cooling liquid according to the degree of thermal fatigue. For this, the main properties of the environment are analyzed, such the chemical composition, corrosion capacity, wetting capacity and cooling characteristics. To analyze the change in properties during the operation, we studied the effect of thermal cycles on the physico-chemical characteristics of the quenching medium to determine the optimal period when the quenching medium could function in good parameters without the necessary corrections. For this purpose, cyclic and linear corrosion tests, FTIR compositional analyses and contact angle measurements were conducted. Full article
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15 pages, 6007 KiB  
Article
The Characterization of a Fragment of a Medieval Fresco from Corbii de Piatră Cave Church
Appl. Sci. 2023, 13(8), 4933; https://doi.org/10.3390/app13084933 - 14 Apr 2023
Cited by 1 | Viewed by 939
Abstract
The fresco of the Corbii de Piatră Cave Church, dating from the end of the 13th century and the beginning of the 14th century, is applied to the sandstone wall. The degradation of the fresco on large surfaces, with many areas of detachment, [...] Read more.
The fresco of the Corbii de Piatră Cave Church, dating from the end of the 13th century and the beginning of the 14th century, is applied to the sandstone wall. The degradation of the fresco on large surfaces, with many areas of detachment, has been determined by the infiltration of meteoric water through the sandstone wall on which it is applied, as well as temperature variations, and repeated wetting/drying processes. However, there are small portions of fresco that show good adhesion to the wall. The present research, aimed at providing scientific data to restorers and historians, involves the advanced characterization of a fragment of fresco with good adhesion to the wall and is being carried out by an interdisciplinary team. The stratigraphy, microstructure, compaction defects, chemical composition, and variation of chemical composition in the fresco from the pictorial surface to the mortar-sandstone interface were determined. Correlations were established between degradation processes and wall adhesion. Full article
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11 pages, 1286 KiB  
Article
The Influence of Brushing Motion on the Cutting Efficiency of Two Heat-Treated Endodontic Files: An In-Vitro Micro Computed Tomography Study
Appl. Sci. 2023, 13(1), 292; https://doi.org/10.3390/app13010292 - 26 Dec 2022
Cited by 1 | Viewed by 985
Abstract
Background: To assess the cutting efficiency of two heat-treated endodontic files with a brushing motion in oval-shaped canals. Methods: A total of 10 intact lower molars with a single oval distal canal were selected and randomly divided into two groups according [...] Read more.
Background: To assess the cutting efficiency of two heat-treated endodontic files with a brushing motion in oval-shaped canals. Methods: A total of 10 intact lower molars with a single oval distal canal were selected and randomly divided into two groups according to the system used for shaping: 2Shape and Hyflex CM. The instrumentation was performed in two parts: a first shaping according to the manufacturer’s instructions and final shaping using 5 brushing motions on the distal, lingual, and buccal walls, avoiding the danger zones. Micro computed tomography (micro-CT) scans before and after the brushing motion were superimposed at all three levels: coronal, middle, and apical. Canal changes in buccolingual (ΔBL) and mesiodistal (ΔMD) dimensions were measured. Data were statistically analyzed by repeated-measures analyses of variance and the student t-test (p < 0.05). Results: For ΔMD, no significant difference emerged between the 2Shape and Hyflex CM in the apical and coronal thirds. However, the cutting efficiency was significantly greater with the 2Shape in the middle third (p < 0.05). Regarding ΔBL, no statistically significant difference was detected between 2Shape and Hyflex CM comparing the anatomical thirds, while 2Shape had a significant higher cutting efficiency considering the total BL diameter (p < 0.05). Conclusions: Under the limits of a vitro study, the shaping procedure with 2Shape and brushing motion was more efficient than the Hyflex CM in the midroot levels in terms of ΔMD, and in total canal space for ΔBL. Both files ensured an effective mechanical preparation. Full article
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20 pages, 9277 KiB  
Article
The Influence of Processing Time on Morphology, Structure and Functional Properties of PEO Coatings on AZ63 Magnesium Alloy
Appl. Sci. 2022, 12(24), 12848; https://doi.org/10.3390/app122412848 - 14 Dec 2022
Cited by 4 | Viewed by 1120
Abstract
The plasma electrolytic oxidation (PEO) surface modification technique was employed for improving the mechanical and anti-corrosion properties of the AZ63 magnesium alloy. Different PEO processing times (5, 10 and 20 min) in a 10 g/L NaAlO2 electrolyte, with no other additives, led to [...] Read more.
The plasma electrolytic oxidation (PEO) surface modification technique was employed for improving the mechanical and anti-corrosion properties of the AZ63 magnesium alloy. Different PEO processing times (5, 10 and 20 min) in a 10 g/L NaAlO2 electrolyte, with no other additives, led to the formation of ceramic coatings with mean thicknesses between 15 and 37 microns. Scanning electron microscopy (SEM) showed that the porosity of the coatings decreased with processing time, but an increase in roughness was observed. X-Ray diffraction phase analysis indicated a coating structure composed of majority magnesium aluminate spinel. The corrosion rate of the coated samples decreased with an order of magnitude compared with the bare alloy. The average micro-hardness values of the PEO-coated samples was up to five times higher than those of the AZ63 alloy. Full article
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16 pages, 4099 KiB  
Article
Hydrophobic Carbonate Coatings on Pure Biodegradable Mg by Immersion in Carbonated Water: Formation Mechanism
Appl. Sci. 2022, 12(22), 11674; https://doi.org/10.3390/app122211674 - 17 Nov 2022
Cited by 2 | Viewed by 1227
Abstract
Mg is one of the few materials of choice for biodegradable implants, despite its rapid degradation when used without surface protection treatment. This study presents the effect of carbonation time on the formation of hydrophobic carbonate coatings grown on pure magnesium using a [...] Read more.
Mg is one of the few materials of choice for biodegradable implants, despite its rapid degradation when used without surface protection treatment. This study presents the effect of carbonation time on the formation of hydrophobic carbonate coatings grown on pure magnesium using a simple, green chemical conversion method in carbonated water. The evolution of the coating with immersion time in carbonating solution was studied in order to ascertain the mechanistic of coating formation by Raman and EDS spectroscopy, XRD, SEM and AFM microscopy. Wettability was investigated by contact angle measurements. The formation mechanism of the hydrophobic coating involves the surface nucleation of carbonates mediated by the dissolution of the native corrosion product, brucite Mg(OH)2, surface conversion into hydroxycarbonates, surface calcite nucleation and growth by attachment of nanoparticles, leading to the lateral growth of a continuous carbonate coating layer of intertwined calcite microcrystals. Full article
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Review

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33 pages, 5128 KiB  
Review
Mineral Characterization Using Scanning Electron Microscopy (SEM): A Review of the Fundamentals, Advancements, and Research Directions
Appl. Sci. 2023, 13(23), 12600; https://doi.org/10.3390/app132312600 - 22 Nov 2023
Viewed by 2563
Abstract
Scanning electron microscopy (SEM) is a powerful tool in the domains of materials science, mining, and geology owing to its enormous potential to provide unique insight into micro and nanoscale worlds. This comprehensive review discusses the background development of SEM, basic SEM operation, [...] Read more.
Scanning electron microscopy (SEM) is a powerful tool in the domains of materials science, mining, and geology owing to its enormous potential to provide unique insight into micro and nanoscale worlds. This comprehensive review discusses the background development of SEM, basic SEM operation, including specimen preparation and image processing, and the fundamental theoretical calculations underlying SEM operation. It provides a foundational understanding for engineers and scientists who have never had a chance to dig in depth into SEM, contributing to their understanding of the workings and development of this robust analytical technique. The present review covers how SEM serves as a crucial tool in mineral characterization, with specific discussion on the workings and research fronts of SEM-EDX, SEM-AM, SEM-MLA, and QEMSCAN. With automation gaining pace in the development of all spheres of technology, understanding the uncertainties in SEM measurements is very important. The constraints in mineral phase identification by EDS spectra and sample preparation are conferred. In the end, future research directions for SEM are analyzed with the possible incorporation of machine learning, deep learning, and artificial intelligence tools to automate the process of mineral identification, quantification, and efficient communication with researchers so that the robustness and objectivity of the analytical process can be improved and the analysis time and involved costs can be reduced. This review also discusses the idea of integrating robotics with SEM to make the equipment portable so that further mineral characterization insight can be gained not only on Earth but also on other terrestrial grounds. Full article
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