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81 pages, 10454 KiB  
Review
Glancing Angle Deposition in Gas Sensing: Bridging Morphological Innovations and Sensor Performances
by Shivam Singh, Kenneth Christopher Stiwinter, Jitendra Pratap Singh and Yiping Zhao
Nanomaterials 2025, 15(14), 1136; https://doi.org/10.3390/nano15141136 - 21 Jul 2025
Viewed by 390
Abstract
Glancing Angle Deposition (GLAD) has emerged as a versatile and powerful nanofabrication technique for developing next-generation gas sensors by enabling precise control over nanostructure geometry, porosity, and material composition. Through dynamic substrate tilting and rotation, GLAD facilitates the fabrication of highly porous, anisotropic [...] Read more.
Glancing Angle Deposition (GLAD) has emerged as a versatile and powerful nanofabrication technique for developing next-generation gas sensors by enabling precise control over nanostructure geometry, porosity, and material composition. Through dynamic substrate tilting and rotation, GLAD facilitates the fabrication of highly porous, anisotropic nanostructures, such as aligned, tilted, zigzag, helical, and multilayered nanorods, with tunable surface area and diffusion pathways optimized for gas detection. This review provides a comprehensive synthesis of recent advances in GLAD-based gas sensor design, focusing on how structural engineering and material integration converge to enhance sensor performance. Key materials strategies include the construction of heterojunctions and core–shell architectures, controlled doping, and nanoparticle decoration using noble metals or metal oxides to amplify charge transfer, catalytic activity, and redox responsiveness. GLAD-fabricated nanostructures have been effectively deployed across multiple gas sensing modalities, including resistive, capacitive, piezoelectric, and optical platforms, where their high aspect ratios, tailored porosity, and defect-rich surfaces facilitate enhanced gas adsorption kinetics and efficient signal transduction. These devices exhibit high sensitivity and selectivity toward a range of analytes, including NO2, CO, H2S, and volatile organic compounds (VOCs), with detection limits often reaching the parts-per-billion level. Emerging innovations, such as photo-assisted sensing and integration with artificial intelligence for data analysis and pattern recognition, further extend the capabilities of GLAD-based systems for multifunctional, real-time, and adaptive sensing. Finally, current challenges and future research directions are discussed, emphasizing the promise of GLAD as a scalable platform for next-generation gas sensing technologies. Full article
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12 pages, 13899 KiB  
Article
The Role of Pores in the Cavitation Erosion of Additively Manufactured Metal: An In Situ Study
by Yuan Song, Zhenhua Wang and Bingyang Ma
Metals 2025, 15(7), 787; https://doi.org/10.3390/met15070787 - 11 Jul 2025
Viewed by 280
Abstract
Additively manufactured (AM) parts have been applied in many areas with the risk of cavitation erosion (CE), and pores are common defects in AM metals. However, the role of pores in CE is still unclear, and a systematic investigation is needed. In this [...] Read more.
Additively manufactured (AM) parts have been applied in many areas with the risk of cavitation erosion (CE), and pores are common defects in AM metals. However, the role of pores in CE is still unclear, and a systematic investigation is needed. In this study, 316L stainless steel was selected as a model material and produced using laser powder bed fusion; the porosity was 6.4%. The morphological evolution of various pores during CE was investigated via electron backscatter diffraction and scanning electron microscopy. It was found that material removal easily occurred around large polygonal pores. The critical size for large polygonal pores was estimated to be between 13 and 20 μm. For narrow pores, concavity first appeared around the pores during CE, and then the narrow pores closed. Small spherical pores with sizes of 3–9 μm showed strong resistance to CE, and no damage occurred within the 60 min CE period. The main reason that different pores played different roles in CE was analyzed. Finally, factors for improving the CE resistance of AM metals were suggested. The research results are helpful for understanding the CE behaviors of AM metals and porous materials. Full article
(This article belongs to the Section Metal Failure Analysis)
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19 pages, 5011 KiB  
Article
One-Step Synthesis AlCo2O4 and Derived “Al” to Double Optimise the Thermal Decomposition Kinetics and Enthalpy of Ammonium Perchlorate
by Kaihua He, Yanzhi Yang, Zhengyi Zhao, Zhiyong Yan and Xuechun Xiao
Colloids Interfaces 2025, 9(3), 28; https://doi.org/10.3390/colloids9030028 - 10 May 2025
Viewed by 483
Abstract
The solution combustion method is widely used because of its simple operation and ability to produce porous structures. The chemical composition and morphological structure of the material can be regulated by different oxidiser-to-fuel ratios (φ). In this work, AlCo2O4 derived [...] Read more.
The solution combustion method is widely used because of its simple operation and ability to produce porous structures. The chemical composition and morphological structure of the material can be regulated by different oxidiser-to-fuel ratios (φ). In this work, AlCo2O4 derived “Al” catalytic materials were successfully synthesised by adjusting the fuel-to-oxidiser ratio using a one-step solution combustion method. On the one hand, the aluminium nanoparticles act as a part of the metal fuel in the composite solid propellant and, at the same time, serve as a catalytic material. In contrast, the thermal decomposition performance of AP was significantly improved by the synergistic catalysis of AlCo2O4. Among the samples prepared under different fuel ratios, considering all aspects (high-temperature decomposition temperature, activation energy, and decomposition heat) comprehensively, the AlCo2O4 prepared with φ = 0.5 had a more excellent catalytic effect on AP thermal decomposition, and the THTD of AP was reduced to 285.4 °C, which is 188.08 °C lower. The activation energy of the thermal decomposition of AP was also significantly reduced (from 296.14 kJ/mol to 211.67 kJ/mol). In addition, the ignition delay time of AlCo2O4-AP/HTPB was drastically shortened to 9 ms from 28 ms after the addition of 7% AlCo2O4 derived “Al” catalytic materials. Composite solid propellants have shown great potential for application. Full article
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16 pages, 12609 KiB  
Article
Microstructure and Micro-Mechanical Properties of Thermally Sprayed HA-TiO2 Coating on Beta-Titanium Substrate
by Abdulaziz Kurdi, Doaa Almalki, Ahmed Degnah and Animesh Kumar Basak
Materials 2025, 18(3), 540; https://doi.org/10.3390/ma18030540 - 24 Jan 2025
Viewed by 998
Abstract
Metallic biomaterials in a solid form cause stress-shielding in orthopedic applications. Such implants also suffer from limited tissue attachment to become a part of the living system. In view of that, hydroxyapatite (HA) coating reinforced with titanium oxide (TiO2) was deposited [...] Read more.
Metallic biomaterials in a solid form cause stress-shielding in orthopedic applications. Such implants also suffer from limited tissue attachment to become a part of the living system. In view of that, hydroxyapatite (HA) coating reinforced with titanium oxide (TiO2) was deposited in a beta (β)-Titanium (Ti-35Nb-7Ta-5Zr) substrate by plasma spray. This allows us to exploit the best of the two materials, namely the relatively low modulus of β-Ti, together with the porous and bone-like structure/composition of the HA to facilitate cell growth. This is foreseen to be used as an implant, particularly for musculoskeletal-related disability. Detailed scanning electron microscopy (SEM) investigation shows the lamellar structure of the coating that is composed of different phases and some porosities. Transmission electron microscopy (TEM) confirms the co-existence of both the amorphous and crystalline phases that build up the coating structure. In situ micro-mechanical tests revealed that the HA-TiO2 coating was low in strength and modules compared to that of the substrate material, together with lower ductility. The yield stress and modulus of elasticity of the coating were about 877 ± 174 MPa and 447 ± 24 MPa, respectively. In contrast, the beta (β)-Ti substrate possesses about 990 ± 85 MPa of yield stress and 259 ± 19 MPa modulus of elasticity. The deformation mechanism was also quite different, where the coating crumbled under compressive loading, featuring limited ductility with cleavage (brittle)-type fracture, and the substrate showed plastic flow of materials in the form of slip/shear planes with extended ductility. Full article
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20 pages, 5732 KiB  
Article
Development of Tailored Porous Ti6Al4V Materials by Extrusion 3D Printing
by Luis Olmos, Ana Silvia González-Pedraza, Héctor Javier Vergara-Hernández, Didier Bouvard, Monserrat Sofía López-Cornejo and Rumualdo Servín-Castañeda
Materials 2025, 18(2), 389; https://doi.org/10.3390/ma18020389 - 16 Jan 2025
Cited by 1 | Viewed by 921
Abstract
Nowadays, metallic bone replacement is in high demand due to different issues, like sicknesses and accidents. Thus, bone implants are fabricated with tailored properties and microstructure for long-term use in the human body. To improve such implants, 3D printing is the most promising [...] Read more.
Nowadays, metallic bone replacement is in high demand due to different issues, like sicknesses and accidents. Thus, bone implants are fabricated with tailored properties and microstructure for long-term use in the human body. To improve such implants, 3D printing is the most promising technique. Therefore, this work aims to evaluate the fabrication of porous materials by extrusion 3D printing of Ti6Al4V. Cylindrical samples were fabricated from pellets for metal injection molding of Ti6Al4V powders, creating hexagonal channels with three different sizes. The densification kinetics was evaluated by dilatometry tests, which enabled following the densification of the samples during the sintering cycle. Subsequently, the samples were characterized by scanning electron microscopy and X-ray computed tomography to analyze their microstructure. Compression tests evaluated the mechanical strength of sintered samples. It was found that the hexagonal shape during printing is better defined as the channel size increases. The results show similar behavior for each of the channel sizes during sintering; however, greater densification is obtained as the channel size decreases. Additionally, microporosity is obtained at the particle level, which is completely interconnected, ensuring the passage of fluids through the entire sample. On the other hand, as the channel size increases, Young’s modulus and yield strength are considerably reduced. The main conclusion is that parts with two scales of porosity can be designed by the 3D printing extrusion process. Full article
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14 pages, 7302 KiB  
Article
An Insight into Chip and Surface Texture Shaping Under Finish Turning of Powder Steels Infiltrated with Tin Bronze
by Kamil Leksycki, Eugene Feldshtein, Larisa Dyachkova, Katarzyna Arkusz, Maciej Ceglewski and Łukasz Czerwiec
Materials 2024, 17(24), 6244; https://doi.org/10.3390/ma17246244 - 20 Dec 2024
Viewed by 628
Abstract
The manufacturing of work parts made of powder (sintered) steels is currently widespread in industry, as it provides minimal processing allowances and high dimensional accuracy, as well as the required properties and unconventional chemical composition. At the same time, their low tensile or [...] Read more.
The manufacturing of work parts made of powder (sintered) steels is currently widespread in industry, as it provides minimal processing allowances and high dimensional accuracy, as well as the required properties and unconventional chemical composition. At the same time, their low tensile or bending strength must be considered a serious disadvantage. In order to minimize these disadvantages, a number of strengthening technologies are used, among which is the infiltration of porous base materials with metal alloys. In this study, the details of finish turning of sintered iron-graphite-based steel infiltrated with tin bronze with molybdenum disulfide addition are considered. Changes in the shape of chips and their geometric features, as well as the 3D parameters and topography features of the surface machined, are presented after finish turning with AH8015 carbide inserts. The cutting speed (vc) and feed rate (f) were used as variable parameters. It was found that when turning the powder steels under study, the chips took the shape of small fragments or element chips, including segmented chips. For quenching steel, the formation of irregular lamellae was observed and for the initial state, a serrated chip was registered. For the initial state, a reduction in Kb values was observed in the range of the vc of 50–100 m/min and f of 0.05–0.075 mm/rev, and for quenching in the range of 225–250 m/min and 0.05–0.075 mm/rev. Compared to the initial state, for quenching, depending on the cutting parameters, a 14% reduction in the chip spreading ratio Kb or an increase from 2 to 32% was registered. For the initial state and quenching, a decrease in the Sp and Sv parameters was achieved in the range of the vc of 200–250 m/min and f of 0.05–0.075 mm/rev, and there was an increase in the range of 50–150 m/min and 0.125–0.15 mm/rev. Compared to the initial state, an increase in the Sz parameter from 10 to 35% was observed for quenching. On the surfaces machined with vc = 50 m/min and f = 0.05 mm/rev, waves and single significant peaks were observed. On the other hand, vc = 250 m/min and f = 0.15 mm/rev provided classical feed tracks in the form of valleys and irregular ridges on the surfaces machined. The test results can be useful in the design and manufacturing of industrial parts made of powder steels. Full article
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11 pages, 1227 KiB  
Article
Sampling and Comparison of Extraction Techniques Coupled with Gas Chromatography–Mass Spectrometry (GC-MS) for the Analysis of Substrates Exposed to Explosives
by Himanshi Upadhyaya, Alexis J. Hecker and John V. Goodpaster
Chemosensors 2024, 12(12), 251; https://doi.org/10.3390/chemosensors12120251 - 29 Nov 2024
Viewed by 1648
Abstract
Explosive-detecting canines (EDCs) show high sensitivity in detecting explosives that they are trained to detect. The ability of canines to detect explosive residues to the parts per trillion level can sometimes result in nuisance alerts. These nuisance alerts can occur when various materials [...] Read more.
Explosive-detecting canines (EDCs) show high sensitivity in detecting explosives that they are trained to detect. The ability of canines to detect explosive residues to the parts per trillion level can sometimes result in nuisance alerts. These nuisance alerts can occur when various materials (i.e., substrates) are exposed to volatile organic compounds (VOCs) present in explosive mixtures, leading to contamination—the unintended absorption or adsorption of VOCs by the substrate. Chemical constituents such as taggant, plasticizer, and residual solvent in explosives are often composed of VOCs that canines are trained on to detect explosives. Composition C-4 (C4) is a common explosive that EDCs are trained to detect and hence is this study’s focus. Common VOCs of interest emitted from C4 include 2,3-dimethyl-2,3-dinitrobutane (DMNB), 2-ethyl-1 hexanol (2E1H), and cyclohexanone. In this study, we developed a protocol for comparing different substrates such as cotton, cardboard, wood, sheet metal, and glass that were exposed to volatiles from C4. 1-bromooctane (1-BO) was used as a single-odor compound to compare the complex odor originating from C4. Triplicates of substrates such as cotton, wood, cardboard, sheet metal, and glass were exposed to 1 g of C4 in a paint can for one week and the substrates were then extracted using various extraction methods such as liquid injection, direct SPME, and headspace analysis coupled with gas chromatography–mass spectrometry. An extraction time study was performed to determine the optimal extraction time for SPME analysis, and it was found to be 20 min. Comparison of extraction methods revealed that SPME surpassed other techniques as DMNB was found on all substrates using SPME. It was observed that porous substrates such as wood and cardboard have a higher retention capacity for volatiles in comparison to non-porous substrates such as sheet metal and glass. Finally, swabbing was evaluated as a sampling technique for the substrates of interest and the extracts were analyzed using the total vaporization–solid phase microextraction (TV-SPME) technique. No volatiles associated with C4 were identified on conducting a GC-MS analysis, suggesting that swabbing is not an ideal technique for analysis of substrates exposed to C4. Full article
(This article belongs to the Special Issue Detection of Volatile Organic Compounds in Complex Mixtures)
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17 pages, 1631 KiB  
Review
Three-Dimensional Printing of Metallic Parts by Means of Fused Filament Fabrication (FFF)
by Irene Buj-Corral, Felip Fenollosa-Artés and Joaquim Minguella-Canela
Metals 2024, 14(11), 1291; https://doi.org/10.3390/met14111291 - 14 Nov 2024
Cited by 2 | Viewed by 1417
Abstract
Obtaining metallic parts via Additive Manufacturing can yield several advantages over using other traditional manufacturing methods such as machining. Material extrusion (MEX) can handle complex shapes with porous structures and, at the present time, much low-end and desktop equipment is available. In the [...] Read more.
Obtaining metallic parts via Additive Manufacturing can yield several advantages over using other traditional manufacturing methods such as machining. Material extrusion (MEX) can handle complex shapes with porous structures and, at the present time, much low-end and desktop equipment is available. In the present work, different industrial and medical applications of metallic Fused Filament Fabrication (FFF) parts are presented. First, an overview of the process, equipment, and of the metal-filled filaments currently available is provided. Then, the properties of parts and different applications are shown. For example, metal-filled filaments with a low metal content that can be used to obtain plastic parts with metallic appearance (with either steel, copper, or bronze), and filaments with a high metallic content allow obtaining metallic parts with high mechanical strength after a sintering operation. The present contribution aims to be an up-to-date panorama for current industrial and medical results and lessons learnt from the application of FFF to obtain metallic parts. Full article
(This article belongs to the Section Additive Manufacturing)
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26 pages, 10663 KiB  
Article
Modelling of Fluid Permeability at the Interface of the Metal-to-Metal Sealing Surface
by Przemysław Jaszak, Jan Oredsson and Rafał Grzejda
Materials 2024, 17(21), 5194; https://doi.org/10.3390/ma17215194 - 24 Oct 2024
Cited by 1 | Viewed by 878
Abstract
This paper presents a method for modelling the permeability of fluid at the interface formed between flat parallel plates and the sharp-edged ridges of a metal gasket. This work was divided into three stages. In the first stage, numerical calculations simulating the deformation [...] Read more.
This paper presents a method for modelling the permeability of fluid at the interface formed between flat parallel plates and the sharp-edged ridges of a metal gasket. This work was divided into three stages. In the first stage, numerical calculations simulating the deformation (compression of the gasket) were performed. The calculations were carried out using thermomechanical static analysis with commercial software. The purpose of these calculations was to determine the contact area of the gasket ridges with the plates, the deformation of the gasket ridges, and the reaction force resulting from the degree of compression of the gasket. In the second part of this work, analytical calculations were performed to estimate the tightness level. The analytical model proposed in this paper was based on Darcy’s equation, simulating fluid flow through a ring-shaped porous layer. The analytical model also took into account the shape of the roughness profile of the sealed surfaces. A mathematical Ausloos–Berman function based on fractal theory was used to represent it. In the last part of this work, experimental tests were carried out to determine the actual fluid permeability and thus verify the numerical and analytical calculations. Full article
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14 pages, 2853 KiB  
Article
The Effect of Epoxy Resin on the Infiltration of Porous Metal Parts Formed through Laser Powder Bed Fusion
by Jibing Chen, Yanfeng Liu, Yong She, Yang Yang, Xinyu Du, Junsheng Yang and Yiping Wu
J. Compos. Sci. 2024, 8(3), 99; https://doi.org/10.3390/jcs8030099 - 11 Mar 2024
Cited by 1 | Viewed by 2365
Abstract
Laser powder bed fusion (L-PBF) additive manufacturing technology can print multi-material parts with multiple functions/properties, and has great potential for working in harsh application environments. However, the metal blank formed by sintering metal powder material with binder added through L-PBF has an obvious [...] Read more.
Laser powder bed fusion (L-PBF) additive manufacturing technology can print multi-material parts with multiple functions/properties, and has great potential for working in harsh application environments. However, the metal blank formed by sintering metal powder material with binder added through L-PBF has an obvious porous structure and insufficient mechanical properties, and few studies have been conducted studying this. In this paper, epoxy resin was used to impregnate the blank of porous metal parts formed by L-PBF with iron-based powder material at a certain temperature, and a cross-linked curing reaction was carried out with three kinds of phenolic resin in different proportions under the action of a curing agent, so as to fill the pores and achieve the desired mechanical properties. The characteristic peaks of each group of epoxy resin were characterized using Fourier transform infrared spectroscopy (FT-IR) and H-nuclear magnetic resonance (1H-NMR) spectrums. The microstructure, decomposition temperature, and residue of four epoxy resin dispersion systems were analyzed with a scanning electron microscope (SEM), a thermal gravimetric analyzer (TGA), and derivative thermogravimetry (DTG). The results show that the density of the porous metal parts was obviously improved, the heat resistance temperature of the parts could reach 350 °C, and the tensile strength of the sample after EP2-1 impregnation was increased by 4–6 times after curing at 160 °C for 6 h. Therefore, the use of an epoxy resin dispersion system can increase the porosity of L-PBF porous metal parts, but can also significantly improve their mechanical properties, which can help them to meet the requirements of applications as model materials, biological materials, and functional materials to provide a feasible solution. Full article
(This article belongs to the Section Metal Composites)
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16 pages, 2845 KiB  
Article
UVC Box: An Effective Way to Quickly Decontaminate Healthcare Facilities’ Wheelchairs
by Cloé Adam, Marius Colin, Romuald Stock, Laurent Weiss and Sophie C. Gangloff
Life 2024, 14(2), 256; https://doi.org/10.3390/life14020256 - 16 Feb 2024
Viewed by 1500
Abstract
Disinfection in the hospital environment remains challenging, especially for wide and structurally complex objects such as beds or wheelchairs. Indeed, the regular disinfection of these objects with chemicals is manually carried out by healthcare workers and is fastidious and time-consuming. Alternative antibacterial techniques [...] Read more.
Disinfection in the hospital environment remains challenging, especially for wide and structurally complex objects such as beds or wheelchairs. Indeed, the regular disinfection of these objects with chemicals is manually carried out by healthcare workers and is fastidious and time-consuming. Alternative antibacterial techniques were thus proposed in the past decades, including the use of naturally antimicrobial UVC. Here, the antibacterial efficiency of a large UVC box built to accommodate wheelchairs was investigated through testing bacterial burden reductions on various parts of a wheelchair, with various support types and with several treatment durations. The results demonstrate a time-dependent antibacterial effect, with a strong burden reduction at only five minutes of treatment (>3-log median reduction in Escherichia coli and Staphylococcus epidermidis). The UVC flux and residual bacterial burden both significantly varied depending on the spatial location on the wheelchair. However, the nature of the support impacted the antibacterial efficiency even more, with residual bacterial burdens being the lowest on rigid materials (steel, plastics) and being the highest on tissue. On metallic samples, the nature of the alloy and surface treatment had various impacts on the antibacterial efficiency of the UVC. This study highlights the efficiency of the tested UVC box to efficiently and quickly decontaminate complex objects such as wheelchairs, but also gives rise to the warning to focus on rigid materials and avoid porous materials in the conception of objects, so as to ensure the efficiency of UVC decontamination. Full article
(This article belongs to the Collection Feature Papers in Microbiology)
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10 pages, 5518 KiB  
Article
Microstructure and Phase Composition Changes in Polymer Fiber-Modified Thermacoat™ Lining Exposed to Contact with Liquid Steel
by Marcin Prochwicz, Malgorzata Pomorska, Lukasz Maj and Jerzy Morgiel
Coatings 2024, 14(2), 183; https://doi.org/10.3390/coatings14020183 - 31 Jan 2024
Cited by 1 | Viewed by 1095
Abstract
Multicomponent clay and cenosphere linings protecting ceramic parts exposed to contact with liquid metal during continuous steel casting (CSC) are intended to diminish thermo-mechanical stresses at the beginning of this process. They are effective in their role, but due to their brittle nature, [...] Read more.
Multicomponent clay and cenosphere linings protecting ceramic parts exposed to contact with liquid metal during continuous steel casting (CSC) are intended to diminish thermo-mechanical stresses at the beginning of this process. They are effective in their role, but due to their brittle nature, parts of them come off during transport or mounting. The admixture of polypropylene fibers into linings helps to alleviate problems with handling such parts, though the interaction of such a modified material with liquid steel should be re-assessed. The present experiment involved the preparation of a crucible with a Thermacoat™ (Vesuvius, Skawina, Poland) lining with the addition of Belmix™ (Belgian Fibers Group NV, Mouscron, Belgium) fibers and filling it with a drop of liquid steel. Next, the crucible was sectioned and the changes in its microstructure and phase composition were investigated with optical, scanning and transmission electron microscopy (OM/SEM/TEM) methods. This showed that the modified lining retained its non-wetting property against the steel of the non-modified material. The part with the lining, being in direct contact with the liquid steel, developed a highly porous layer filled with AlSiOx amorphous flakes with some larger blocky Al2O3 and SiO2 particles. Right below this, a heat-affected zone (HAZ) consisting of fine γ-Al2O3 platelets immersed in amorphous silica was formed. Some of the voids with a size corresponding to polymer fiber diameter carried significant carbon deposits on their walls. The performed investigation indicated that the polymer fiber-modified linings were capable of withstanding at least short-term contact with liquid steel without instantaneous defragmentation, i.e., they retained the good high-temperature properties of the non-modified material. Full article
(This article belongs to the Section Functional Polymer Coatings and Films)
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20 pages, 3801 KiB  
Article
Isotopic Tracer Study of Initiation of Porosity in Anodic Alumina Formed in Chromic Acid
by Aleksandra Baron-Wiechec and Guocong Lin
Nanomaterials 2024, 14(1), 42; https://doi.org/10.3390/nano14010042 - 22 Dec 2023
Cited by 1 | Viewed by 1270
Abstract
In this paper, we focused on the initiation of porosity in the anodic alumina under galvanostatic conditions in chromic acid, using an 18O isotope tracer. The general concept of the initiation and growth of porous anodic oxide films on metals has undergone [...] Read more.
In this paper, we focused on the initiation of porosity in the anodic alumina under galvanostatic conditions in chromic acid, using an 18O isotope tracer. The general concept of the initiation and growth of porous anodic oxide films on metals has undergone constant development over many years. A mechanism of viscous flow of the oxide from the barrier layer to the pore walls has recently been proposed. In this work, two types of pre-formed oxide films were analysed: pure Al2O3 formed in chromic acid, and a film containing As ions formed in a sodium arsenate solution. Both were anodized in chromic acid for several different time durations. Both pre-formed films contained the oxygen isotope 18O. The locations and quantities of 18O and As were analysed by means of ion accelerator-based methods supported by transmission electron microscopy. The significant difference observed between the two oxide films is in the 18O distribution following the second step of anodization, when compared with galvanostatic anodization in phosphoric or sulfuric acid reported in previous works. From the current experiment, it is evident that a small amount of As in the pre-formed barrier layer appears to alter the ionic conductivity of the film; thus, somehow, it inhibits the movement of oxygen ions ahead of advancing pores during anodization in chromic acid. However, anodising pure alumina film under these conditions does not enhance oxygen movement within the oxide layer. In addition, the tracer stays in the outer part of the growing porous oxide film. A lower-than-expected value for pure alumina enrichment in 18O in the pre-formed films suggests, indirectly, that the pre-formed film may contain hydrogen species, as well as trapped electrons, since no Cr is detected. This may lead to the presence of space charge distribution, which has a dual effect: it both retards the ejection of Al3+ ions and prevents O2− ions from migrating inward. Thus, the negative- and positive-charge distributions might play a role in the initiation of pores via a flow mechanism. Full article
(This article belongs to the Special Issue Nano-Structured Thin Films: Growth, Characteristics, and Application)
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17 pages, 5840 KiB  
Article
Swift Removal of the Heavy Metals Cadmium and Lead from an Aqueous Solution by a CAN-Zeolite Synthesized from Natural Clay
by Lobna Aloui, Soumaya Mezghich, Lamjed Mansour, Sana Hraiech and Fadhila Ayari
ChemEngineering 2023, 7(6), 113; https://doi.org/10.3390/chemengineering7060113 - 30 Nov 2023
Cited by 5 | Viewed by 2437
Abstract
CAN-zeolite was synthesized with a high purity from natural kaolinite via alkali fusion by hydrothermal treatment at a pressure of 1 kbar H2O. It was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy and nitrogen adsorption at 77 [...] Read more.
CAN-zeolite was synthesized with a high purity from natural kaolinite via alkali fusion by hydrothermal treatment at a pressure of 1 kbar H2O. It was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy and nitrogen adsorption at 77 K. The results show that after AK hydrothermal treatment (under specific conditions), the SBET increases from 5.8 m2g−1 to 30.07 m2g−1 which is six times greater. The AK which was a non-porous or macroporous solid (the nitrogen adsorption/desorption of AK is of type II) became mesoporous (N2 adsorption–desorption isotherms exhibit typical hysteresis of type IV) with a pore size of 5.9 Å. XRD of AK shows the presence of quartz (Q) as impurities, and illite and kaolinite as major fractions; after hydrothermal treatment, the XRD diffractogram shows only fine pics related to CAN-zeolite (with a good crystallinity), confirming the success of the synthesized process. These results suggest that the synthesized CAN-zeolite has the potential to be tested in the removal of heavy metals from waste water as part of a remediation process. Batch reactors were used to evaluate the adsorption isotherms and kinetic studies of heavy metals, cadmium, and lead, by natural kaolinite clay (AK) and synthesized cancrinite zeolite (CAN-zeolite). The results show that the adsorption kinetics of the bivalent heavy metals cadmium and lead are extremely fast with either AK or CAN-zeolite. Equilibrium was reached within 2 min. Adsorption isotherms show that the synthesized CAN-zeolite has a higher adsorption capacity; the retention capacity of lead and cadmium was three times greater than that presented by the natural clay mineral. According to the findings, CAN-zeolite has a higher affinity for PbII (192 mg/g) compared to CdII (68 mg/g). The negative reactive surface sites interacting with these cationic heavy metals resulted in a higher amount of heavy metals adsorption than the cation exchange capacity (CEC). The adsorption information was analyzed using the Langmuir and Freundlich equations. The Langmuir model provided a good fit to the equilibrium data, indicating a monolayer adsorption mechanism. Full article
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18 pages, 5825 KiB  
Review
Research Progress on Metal–Organic Framework-Based Electrode Materials for Supercapacitors
by Yin Zhu, Peng Su, Jiemin Wang and Xu Wang
Crystals 2023, 13(11), 1593; https://doi.org/10.3390/cryst13111593 - 17 Nov 2023
Cited by 14 | Viewed by 4167
Abstract
Supercapacitors play an important role in power systems since they are a key part of electrochemical energy storage devices. To assemble high-performance supercapacitors, it is crucial to discover and innovate high-capacitive electrode materials. Recently, metal–organic frameworks (MOFs) and their derivatives have received wide [...] Read more.
Supercapacitors play an important role in power systems since they are a key part of electrochemical energy storage devices. To assemble high-performance supercapacitors, it is crucial to discover and innovate high-capacitive electrode materials. Recently, metal–organic frameworks (MOFs) and their derivatives have received wide concerns as electrode materials for supercapacitors, not only because of their high pore volume and large surface area for ions and electrons insertion and transportation, but also due to the intrinsic metal active sites that possibly offer extra faradaic pseudocapacitance. Additionally, the abundant species of MOFs with various morphologies also feature advantages in enriching the structural diversity of electrodes. In this paper, we first report the latest research progress and demonstrate the feasibility of pure MOFs for directly constructing supercapacitor electrodes. Furthermore, different MOF derivatives, including porous carbons, transition metal oxides, metal hydroxides and MOF composites for supercapacitors, are summarized, and their electrochemical performances with corresponding energy storage mechanisms are presented in detail. Finally, the perspectives for MOF-based materials applied in supercapacitors are discussed, aiming to provide a guideline for further research based on these promising materials. Full article
(This article belongs to the Special Issue Supercapacitor and Related Materials)
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