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Journal = Micro
Section = Microscale Materials Science

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54 pages, 11611 KiB  
Review
The Quest Towards Superhydrophobic Cellulose and Bacterial Cellulose Membranes and Their Perspective Applications
by Iliana Ntovolou, Despoina Farkatsi and Kosmas Ellinas
Micro 2025, 5(3), 37; https://doi.org/10.3390/micro5030037 (registering DOI) - 31 Jul 2025
Abstract
Over the last few decades, the growing demand for sustainable resources has made biopolymers increasingly popular, as they offer an eco-friendly alternative to conventional synthetic polymers, which are often associated with environmental issues such as the formation of microplastics and toxic substances. Functionalization [...] Read more.
Over the last few decades, the growing demand for sustainable resources has made biopolymers increasingly popular, as they offer an eco-friendly alternative to conventional synthetic polymers, which are often associated with environmental issues such as the formation of microplastics and toxic substances. Functionalization of biomaterials involves modifying their physical, chemical, or biological properties to improve their performance for specific applications. Cellulose and bacterial cellulose are biopolymers of interest, due to the plethora of hydroxyl groups, their high surface area, and high porosity, which makes them ideal candidates for several applications. However, there are applications, which require precise control of their wetting properties. In this review, we present the most effective fabrication methods for modifying both the morphology and the chemical properties of cellulose and bacterial cellulose, towards the realization of superhydrophobic bacterial cellulose films and surfaces. Such materials can find a wide variety of applications, yet in this review we target and discuss applications deriving from the wettability control, such as antibacterial surfaces, wound healing films, and separation media. Full article
(This article belongs to the Section Microscale Materials Science)
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14 pages, 6801 KiB  
Article
Effect of Zr Doping on BNT–5BT Lead-Free Ceramics: Substitutional and Excess Incorporation Analysis
by Mauro Difeo, Miriam Castro and Leandro Ramajo
Micro 2025, 5(3), 35; https://doi.org/10.3390/micro5030035 - 28 Jul 2025
Viewed by 86
Abstract
This study evaluates the effect of zirconium (Zr) incorporation on the structural, microstructural, and functional properties of lead-free ceramics based on the 0.95(Bi0.5Na0.5)TiO3–0.05BaTiO3 (BNT–5BT) system. Two distinct doping strategies were investigated: (i) the substitutional incorporation of [...] Read more.
This study evaluates the effect of zirconium (Zr) incorporation on the structural, microstructural, and functional properties of lead-free ceramics based on the 0.95(Bi0.5Na0.5)TiO3–0.05BaTiO3 (BNT–5BT) system. Two distinct doping strategies were investigated: (i) the substitutional incorporation of Zr4+ at the Ti4+ site (BNT–5BT–xZrsub), and (ii) the addition of ZrO2 in excess (BNT–5BT–xZrexc). The samples were synthesized via conventional solid-state reaction and characterized using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM/EDS), and electrical measurements, including dielectric, ferroelectric, and piezoelectric responses. Both doping routes were found to influence phase stability and electromechanical performance. Substitutional doping notably reduced the coercive field while preserving high remanent polarization, resulting in an enhanced piezoelectric coefficient (d33). These results highlight the potential of Zr-modified BNT–5BT ceramics for lead-free energy harvesting applications. Full article
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14 pages, 4290 KiB  
Article
Multifunctional Green-Synthesized Cu2O-Cu(OH)2 Nanocomposites Grown on Cu Microfibers for Water Treatment Applications
by Hala Al-Jawhari, Nuha A. Alhebshi, Roaa Sait, Reem Altuwirqi, Laila Alrehaili, Noorah Al-Ahmadi and Nihal Elbialy
Micro 2025, 5(3), 33; https://doi.org/10.3390/micro5030033 - 5 Jul 2025
Viewed by 337
Abstract
Free-standing copper oxide (Cu2O)-copper hydroxide (Cu(OH)2) nanocomposites with enhanced catalytic and antibacterial functionalities were synthesized on copper mesh using a green method based on spinach leaf extract and glycerol. EDX, SEM, and TEM analyses confirmed the chemical composition and [...] Read more.
Free-standing copper oxide (Cu2O)-copper hydroxide (Cu(OH)2) nanocomposites with enhanced catalytic and antibacterial functionalities were synthesized on copper mesh using a green method based on spinach leaf extract and glycerol. EDX, SEM, and TEM analyses confirmed the chemical composition and morphology. The resulting Cu2O-Cu(OH)2@Cu mesh exhibited notable hydrophobicity, achieving a contact angle of 137.5° ± 0.6, and demonstrated the ability to separate thick oils, such as HD-40 engine oil, from water with a 90% separation efficiency. Concurrently, its photocatalytic performance was evaluated by the degradation of methylene blue (MB) under a weak light intensity of 5 mW/cm2, achieving 85.5% degradation within 30 min. Although its application as a functional membrane in water treatment may raise safety concerns, the mesh showed significant antibacterial activity against both Gram-positive (Staphylococcus aureus) and Gram-negative (Escherichia coli) bacteria under both dark and light conditions. Using the disk diffusion method, strong bacterial inhibition was observed after 24 h of exposure in the dark. Upon visible light irradiation, bactericidal efficiency was further enhanced—by 17% for S. aureus and 2% for E. coli. These findings highlight the potential of the Cu2O-Cu(OH)2@Cu microfibers as a multifunctional membrane for industrial wastewater treatment, capable of simultaneously removing oil, degrading organic dyes, and inactivating pathogenic bacteria through photo-assisted processes. Full article
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13 pages, 5678 KiB  
Article
Automated SILAR System for High-Precision Deposition of CZTS Semiconductor Thin Films
by Perla J. Vázquez-González, Martha L. Paniagua-Chávez, Rafael Mota-Grajales and Carlos A. Hernández-Gutiérrez
Micro 2025, 5(3), 32; https://doi.org/10.3390/micro5030032 - 24 Jun 2025
Viewed by 272
Abstract
In this work, we present the development and validation of an automated system for the Successive Ionic Layer Adsorption and Reaction (SILAR) method, aimed at depositing Cu2ZnSnS4 (CZTS) thin films. The system is based on a Raspberry Pi Pico microcontroller [...] Read more.
In this work, we present the development and validation of an automated system for the Successive Ionic Layer Adsorption and Reaction (SILAR) method, aimed at depositing Cu2ZnSnS4 (CZTS) thin films. The system is based on a Raspberry Pi Pico microcontroller programmed in Micro-Python (Thonny 4.0.2), allowing precise control over immersion sequences, timing intervals, and substrate positioning along two degrees of freedom. Automation enhances reproducibility, safety, and reduces human error compared with manual operation. CZTS films were deposited on borosilicate glass and optically and structurally characterized. A gradual darkening of the films with increasing deposition cycles indicates controlled material accumulation. X-ray diffraction (XRD) and Raman spectroscopy confirmed the presence of CZTS phases, although with a partially amorphous structure. The estimated optical bandgap of ~1.34 eV is consistent with photovoltaic applications. These results validate the functionality of the automated SILAR platform for repeatable and scalable thin-film fabrication, offering a low-cost alternative for producing semiconductor absorber layers in solar energy technologies. Full article
(This article belongs to the Section Microscale Materials Science)
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18 pages, 3043 KiB  
Article
Fe-Doped ZnS Quantum Dot Photocatalysts for the Degradation of Cefalexin in Water
by Sonia J. Bailon-Ruiz, Yarilyn Cedeño-Mattei and Luis Alamo-Nole
Micro 2025, 5(3), 31; https://doi.org/10.3390/micro5030031 - 22 Jun 2025
Viewed by 295
Abstract
This study reports the synthesis, structural characterization, adsorption studies, nanoscale interaction, and photocatalytic application of pure and Fe-doped ZnS quantum dots for the degradation of the antibiotic cefalexin in aqueous solution. Nanoparticles were synthesized via the microwave-assisted method, and Fe doping was introduced [...] Read more.
This study reports the synthesis, structural characterization, adsorption studies, nanoscale interaction, and photocatalytic application of pure and Fe-doped ZnS quantum dots for the degradation of the antibiotic cefalexin in aqueous solution. Nanoparticles were synthesized via the microwave-assisted method, and Fe doping was introduced at a 1% molar ratio. HRTEM images confirmed quasi-spherical morphology and high crystallinity, with particle sizes averaging 2.4 nm (pure) and 3.5 nm (doped). XRD analysis showed a consistent cubic ZnS structure. UV-vis spectra showed strong absorption at 316 nm for both samples, and PL measurements revealed emission quenching upon Fe doping. Photocatalytic tests under UV light demonstrated significantly higher degradation rates of 10 ppm cefalexin with Fe-doped ZnS, reaching near-complete removal within 90 min. Adsorption experiments revealed higher affinity and adsorption capacity of Fe-doped ZnS toward cefalexin compared to pure ZnS, as demonstrated by the Freundlich isotherm analyses, contributing significantly to enhanced photocatalytic degradation performance. High-resolution QTOF LC-MS analysis confirmed the breakdown of the β-lactam and thiazolidine rings of cefalexin and the formation of low-mass degradation products, including fragments at m/z 122.0371, 116.0937, and 318.2241. These findings provide strong evidence for the structural destruction of the antibiotic and validate the enhanced photocatalytic performance of Fe-doped ZnS. Full article
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15 pages, 2458 KiB  
Article
High-Performance EMI Shielding Film Based on Low-Dk Polyimide and Trimodal Ag Ink for High-Speed Signal Integrity Enhancement
by Moses Gu, Suin Chae, Seonwoo Kim, Yubin Kim, Shinui Kang, Soobin Park, Se-Hoon Park, Sung-Hoon Choa and Hyunjin Nam
Micro 2025, 5(2), 26; https://doi.org/10.3390/micro5020026 - 28 May 2025
Viewed by 1077
Abstract
Electromagnetic interference (EMI) shielding is critical for maintaining signal integrity in high-speed electronic packaging. However, conventional shielding approaches face limitations in process complexity and spatial efficiency. In this study, an EMI shielding film based on trimodal silver (Ag) ink and low-dielectric polyimide (PI) [...] Read more.
Electromagnetic interference (EMI) shielding is critical for maintaining signal integrity in high-speed electronic packaging. However, conventional shielding approaches face limitations in process complexity and spatial efficiency. In this study, an EMI shielding film based on trimodal silver (Ag) ink and low-dielectric polyimide (PI) resin was developed and comprehensively evaluated. The fabricated film exhibited an average shielding effectiveness (SE) of −99.7 dB in the 6–18 GHz frequency range and demonstrated a 50% increase in electrical conductivity after lamination (from 0.752 × 105 S/m to 1.13 × 105 S/m). The horizontal thermal conductivity reached 34.614 W/m·K, which was 3.4 times higher than the vertical value (10.249 W/m·K). Signal integrity simulations showed significant reductions in near-end crosstalk (NEXT, 77.8%) and far-end crosstalk (FEXT, 65%). Moreover, cyclic bending tests confirmed excellent mechanical durability, with a normalized resistance change below 0.6 after 1000 cycles at a bending radius of 4 mm. Notably, the film enabled a 50% reduction in signal line spacing while maintaining signal integrity, even without strict compliance with the 3W Rule. These results demonstrate the potential of the proposed EMI shielding film as a high-performance solution for advanced packaging applications requiring high-frequency operation, thermal management, and mechanical flexibility. Full article
(This article belongs to the Section Microscale Materials Science)
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17 pages, 5425 KiB  
Article
Fine-Tuning Flexographic Ink’s Surface Properties and Providing Anti-Counterfeit Potential via the Addition of TiO2 and ZnO Nanoparticles
by Tamara Tomašegović, Sanja Mahović Poljaček, Ivona Jurišić and Davor Donevski
Micro 2025, 5(2), 20; https://doi.org/10.3390/micro5020020 - 28 Apr 2025
Viewed by 419
Abstract
The objective of this research was to fine-tune the surface properties of printed ink layers by incorporating TiO2 and ZnO nanoparticles into conventional flexographic ink. This modification aimed to improve print quality while simultaneously providing protection against counterfeiting. The presence of nanoparticles [...] Read more.
The objective of this research was to fine-tune the surface properties of printed ink layers by incorporating TiO2 and ZnO nanoparticles into conventional flexographic ink. This modification aimed to improve print quality while simultaneously providing protection against counterfeiting. The presence of nanoparticles in the inks was indirectly detected through FTIR-ATR spectroscopy, which revealed changes in the fingerprint region of the ink spectrum when nanoparticles were added. This alteration enhanced the anti-counterfeiting potential of a produced print. The colorimetric measurements indicated that the addition of nanoparticles did not significantly affect the colorimetric properties of the print, since the maximal calculated ΔEab value was 2.83. However, the nanoparticles notably improved the ink coverage on printed line elements and allowed for the printing of elements without the characteristic outline associated with flexographic printing. The best results in terms of line definition and coverage were achieved with the addition of 2% rutile TiO2 and 1% ZnO to the ink: the measured line segment area covered in ink was 28.5% larger than the same area printed using unmodified ink. This improvement in print quality was attributed to the modified surface free energy (SFE) of the inks, which also influenced the adhesion parameters between the printed layer and the printing substrate. The lowest total SFE was calculated for the ink without added nanoparticles (40.31 mJ/m2), and the highest for the ink with the addition of 2% rutile TiO2 (48.33 mJ/m2). The work of adhesion increased after adding the nanoparticles to the ink, thereby improving the adhesion. The highest work of adhesion (79.36 mJ/m2) was calculated for the ink with 2% rutile TiO2. Interfacial tension was low and close to zero for all printed ink layers, and the lowest value was achieved for the ink without added nanoparticles (1.47 mJ/m2). The findings of this research demonstrated that fine-tuning the properties of flexographic inks using nanoparticles can yield several benefits in terms of optimizing the quality of and providing counterfeit protection for specific printed motifs. Full article
(This article belongs to the Section Microscale Materials Science)
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22 pages, 2510 KiB  
Article
Roles of Polymerization Temperature and Initiator Type on Thermal Properties of Rubitherm® 21 PCM Microcapsules
by Refat Al-Shannaq, Monzer Daoud, Mohammed Farid, Md Wasi Ahmad, Shaheen A. Al-Muhtaseb, Mazhar Ul-Islam, Abdullah Al Saidi and Imran Zahid
Micro 2025, 5(2), 19; https://doi.org/10.3390/micro5020019 - 12 Apr 2025
Viewed by 1393
Abstract
Thermal energy storage offers a viable solution for managing intermediate energy availability challenges. Phase change materials (PCMs) have been extensively studied for their capacity to store thermal energy when available and release it when needed, maintaining a narrow temperature range. However, effective utilization [...] Read more.
Thermal energy storage offers a viable solution for managing intermediate energy availability challenges. Phase change materials (PCMs) have been extensively studied for their capacity to store thermal energy when available and release it when needed, maintaining a narrow temperature range. However, effective utilization of PCMs requires its proper encapsulation in most applications. In this study, microcapsules containing Rubitherm®(RT) 21 PCM (Tpeak = 21 °C, ΔH = 140 kJ/kg), which is suitable for buildings, were synthesized using a suspension polymerization technique at different operating temperatures (45–75 °C). Two different water-insoluble thermal initiators were evaluated: 2,2-Azobis (2,4-dimethyl valeronitrile) (Azo-65) and benzoyl peroxide (BPO). The prepared microcapsules were characterized using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), particle size distribution (PSD), scanning electron microscope (SEM), and optical microscopy (OM). Additionally, the microcapsules were subjected to multiple melting and freezing cycles to assess their thermal reliability and performance stability. DSC results revealed that the microcapsules using BPO exhibited a latent heat of melting comparable to those produced with Azo-65 at an operating temperature of 75 °C. However, the onset crystallization temperature for the BPO-encapsulated PCMs was approximately 2 °C lower than that of the Azo-65-encapsulated PCMs. The greatest latent heat of melting, 107.76 J/g, was exhibited by microcapsules produced at 45 °C, representing a PCM content of 82 wt. %. On the other hand, microcapsules synthesized at 55 °C and 75 °C showed latent heats of 96.02 J/g and 95.66 J/g, respectively. The degree of supercooling for PCM microcapsules was reduced by decreasing the polymerization temperature, with the lowest supercooling observed for microcapsules synthesized at 45 °C. All microcapsules exhibited a monodisperse and narrow PSD of ~10 µm, indicating uniformity in microcapsule size and demonstrating that temperature variations had no significant impact on the particle size distribution. Future research should focus on low-temperature polymerization with extended polymerization times. Full article
(This article belongs to the Section Microscale Materials Science)
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15 pages, 4670 KiB  
Article
Microwave-Assisted Carbonization Processing for Carbon Dot-like Nanomaterials with Antimicrobial Properties
by Buta Singh, Audrey F. Adcock, Simran Dumra, Jordan Collins, Liju Yang, Christopher E. Bunker, Haijun Qian, Mohammed J. Meziani and Ya-Ping Sun
Micro 2025, 5(1), 14; https://doi.org/10.3390/micro5010014 - 17 Mar 2025
Cited by 2 | Viewed by 1258
Abstract
Carbon dots (CDots) are classically defined as small carbon nanoparticles with effective surface passivation, which, in the classical synthesis, has been accomplished by surface organic functionalization. CDot-like nanostructures could also be produced by the thermal carbonization processing of selected organic precursors, in which [...] Read more.
Carbon dots (CDots) are classically defined as small carbon nanoparticles with effective surface passivation, which, in the classical synthesis, has been accomplished by surface organic functionalization. CDot-like nanostructures could also be produced by the thermal carbonization processing of selected organic precursors, in which the non-molecular nanocarbons resulting from the carbonization are embedded in the remaining organic species, which may provide the passivation function for the nanocarbons. In this work, a mixture of oligomeric polyethylenimine and citric acid in the solid state was used for efficient thermal carbonization processing with microwave irradiation under various conditions to produce dot samples with different nanocarbon content. The samples were characterized in terms of their structural and morphological features regarding their similarity or equivalency to those of the classical CDots, along with their significant divergences. Also evaluated were their optical spectroscopic properties and their photoinduced antimicrobial activity against selected bacterial species. The advantages and disadvantages of the thermal carbonization processing method and the resulting dot samples with various features and properties mimicking those of classically synthesized CDots are discussed. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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14 pages, 4498 KiB  
Article
Chemical Synthesis of Nanostructured Topological Pb1−xSnxSe (x = 0–1) Alloy Films—A Study of Their Structural, Optical, and Thermopower Properties
by Esteban Díaz-Torres, Ángel Guillén-Cervantes and Mauricio Ortega-López
Micro 2025, 5(1), 13; https://doi.org/10.3390/micro5010013 - 16 Mar 2025
Viewed by 745
Abstract
The spray pyrolysis deposition of nanostructured Pb1−xSnxSe alloy films, x = 0.0 to 1.0, from as-prepared Pb1−xSnxSe alloy colloids as the starting solution is reported. The colloidal dispersions were prepared by dissolving selenium [...] Read more.
The spray pyrolysis deposition of nanostructured Pb1−xSnxSe alloy films, x = 0.0 to 1.0, from as-prepared Pb1−xSnxSe alloy colloids as the starting solution is reported. The colloidal dispersions were prepared by dissolving selenium in an amine–thiol mixture, reacted with the Sn and Pb precursors in propylene glycol, and subsequently sprayed onto glass substrates at 300 °C. Structural characterization indicated the formation of the alloyed rock-salt cubic phase for 0.0 ≤ x ≤ 0.75, oxidized Pb and Se phases produced during the deposition, and only orthorhombic SnSe for x = 1.0 with Se and SnSe2 as impurities. Nanocrystalline films ranging from 16 to 16.5 nm in size were obtained. The films displayed a shift in their optical structure and a non-monotonic variation in the band gap energy, first a decrease, reaching the minimum at x = 0.30 and a further increase in the Sn content. The decrease in the optical band gap resembles that of a topological insulator behavior. The morphology of the alloyed films confirmed the large nanocrystal formation by self-assembly processes in both the PbSe and SnSe phases and segregated PbSnSe platelets for x ≥ 0.30. Seebeck coefficient revealed that a typical semiconductor behavior dominated by bipolar transport, and p-type conductivity, but only for x = 0.0 n-type conductivity was exhibited. The maximal Seebeck coefficient magnitude behaved similarly to the band gap energy, evidencing the influence of energy band structure and the topological character. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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28 pages, 17094 KiB  
Article
Innovative Elaboration of Polyvinylidene Fluoride Thin Films via Dip-Coating: Beta Phase Optimization, Humidity Control, Nanoparticles Addition, and Topographic Analysis
by Marwan Fakhry, Olivier Soppera and Dominique Berling
Micro 2025, 5(1), 12; https://doi.org/10.3390/micro5010012 - 14 Mar 2025
Cited by 1 | Viewed by 1590
Abstract
Polyvinylidene fluoride (PVDF) is a multifunctional polymer renowned for its unique electrical, mechanical, and piezoelectric properties, making it an attractive candidate for various applications. Although the spin-coating method has been the conventional method for fabricating PVDF thin films, this work is the first [...] Read more.
Polyvinylidene fluoride (PVDF) is a multifunctional polymer renowned for its unique electrical, mechanical, and piezoelectric properties, making it an attractive candidate for various applications. Although the spin-coating method has been the conventional method for fabricating PVDF thin films, this work is the first to apply the dip-coating technique with humidity control, which is a largely unexplored method in the literature on PVDF thin films. This novel approach offers great prospects for improved control and performance adjustments, as well as expanding the range of film deposition procedures. Here, we examine the phase composition of PVDF thin films; adjust different parameters to optimize the electroactive phases fraction, especially the Beta phase; and examine how relative humidity affects the properties of the film. Moreover, we test the impact of different nanoparticles’ addition on the phases fraction and characteristics of the film. Furthermore, we analyze the topography of the resultant films using several approaches, providing fresh insights into their structural features. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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13 pages, 2167 KiB  
Article
Development of Quercetin Micellar Nanogel: Formulation, Characterization, and In Vitro Cytotoxocity Study
by Harshad S. Kapare, Sunil Kanadje, Prabhanjan Giram, Aditi Patil and Ritesh P. Bhole
Micro 2025, 5(1), 6; https://doi.org/10.3390/micro5010006 - 30 Jan 2025
Viewed by 1592
Abstract
Quercetin, a flavonoid, has well-proven cytotoxicity potential, but its therapeutic efficacy is hampered by hydrophobicity, stability issues, and lower bioavailability. The present research aims to address these issues and formulation barriers by formulating a quercetin-loaded micellar nanogel. Quercetin was encapsulated in PF 68 [...] Read more.
Quercetin, a flavonoid, has well-proven cytotoxicity potential, but its therapeutic efficacy is hampered by hydrophobicity, stability issues, and lower bioavailability. The present research aims to address these issues and formulation barriers by formulating a quercetin-loaded micellar nanogel. Quercetin was encapsulated in PF 68 micelles to enhance its solubility, loading, and stability to better its therapeutic potential. The nanogel was further characterized regarding for pH, spreadability, and in vitro cytotoxicity against human breast cancer cells (MCF-7). The resulting micelles exhibited a particle size of 180.26 ± 2.4 nm, surface charge of −13.5 mV, entrapment efficiency of 78.4 ± 1.2%, and in vitro release of 96.11 ± 0.75% up to 8 h. This in vitro cytotoxicity study on MCF-7 cell lines reveals the improved TGI and GI 50 values of micellar nanogel formulation compared to quercetin. The overall study results demonstrated that the developed micellar nanogel system might serve as a promising nanocarrier to enhance the cytotoxic potential of quercetin in cancer therapy. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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12 pages, 3038 KiB  
Article
Strong Electronic Interaction Between Oxygen Vacancy-Enriched Cobalt-Oxide Support and Nickel-Hydroxide Nanoparticles for Enhanced CO Production
by Dinesh Bhalothia, Tien-Fu Li, Amisha Beniwal, Ashima Bagaria and Tsan-Yao Chen
Micro 2025, 5(1), 4; https://doi.org/10.3390/micro5010004 - 26 Jan 2025
Cited by 1 | Viewed by 906
Abstract
The catalytic conversion of carbon dioxide (CO2) into carbon monoxide (CO) via the reverse water–gas shift (RWGS) reaction offers a promising pathway toward a sustainable carbon cycle. However, the competing Sabatier reaction presents a significant challenge, underscoring the need for highly [...] Read more.
The catalytic conversion of carbon dioxide (CO2) into carbon monoxide (CO) via the reverse water–gas shift (RWGS) reaction offers a promising pathway toward a sustainable carbon cycle. However, the competing Sabatier reaction presents a significant challenge, underscoring the need for highly efficient catalysts. In this study, we developed a novel catalyst comprising cobalt-oxide-supported nickel-hydroxide nanoparticles (denoted as Co@Ni). This catalyst achieved a remarkable CO production yield of ~5144 μmol g−1 at 573 K, with a CO selectivity of 77%. These values represent 30% and 70% improvements over carbon-supported Ni(OH)2 (Ni-AC) and CoO (Co-AC) nanoparticles, respectively. Comprehensive physical characterizations and electrochemical analyses reveal that the exceptional CO yield of the Co@Ni catalyst stems from the synergistic electronic interactions between adjacent active sites. Specifically, cobalt-oxide domains act as electron donors to Ni sites, facilitating efficient H2 splitting. Additionally, the oxygen vacancies in cobalt oxide enhance CO2 adsorption and promote subsequent dissociation. These findings provide critical insights into the design of highly efficient and selective catalysts for the RWGS reaction, paving the way for advancements in sustainable carbon utilization technologies. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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13 pages, 2247 KiB  
Article
Controlled Hydrogen Loading of Magnesium Thin Films in KOH—Effects on the Hydride Nucleation and Growth Regimes
by Giorgia Guardi, Angelina Sarapulova, Sonia Dsoke, Stefan Wagner, Luca Pasquini and Astrid Pundt
Micro 2024, 4(4), 765-777; https://doi.org/10.3390/micro4040047 - 5 Dec 2024
Cited by 1 | Viewed by 1206
Abstract
In this work, we propose a strategy to optimize electrochemical hydrogen loading in magnesium–palladium thin films, using 5 M KOH as an electrolyte. Mg thin films of thickness 26 nm were deposited on sapphire (0001) substrates and capped by a 32 nm Pd [...] Read more.
In this work, we propose a strategy to optimize electrochemical hydrogen loading in magnesium–palladium thin films, using 5 M KOH as an electrolyte. Mg thin films of thickness 26 nm were deposited on sapphire (0001) substrates and capped by a 32 nm Pd layer. By performing cyclic voltammetry with in situ optical microscopy, it appears that a loading potential of at least −1.2 V vs. Hg/HgO has to be achieved at the sample’s surface to trigger magnesium hydride formation. Loading potential effects are then further explored by hydrogenography, where different hydride formation mechanisms appear based on the actual potential. With a larger loading potential of −1.6 V vs. Hg/HgO, a magnesium hydride blocking layer is formed; in this case, Pd hydride temporarily forms in the capping layer as hydrogen diffuses towards the magnesium layer. Loading is optimized for a lower potential of −1.2 V vs. Hg/HgO, which leads to larger hydride precipitates and delays the blocking layer formation; in this case, Pd hydride only appears after the magnesium layer is completely hydrided. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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14 pages, 21628 KiB  
Article
Oxidation Behavior and Creep Resistance of Cast MC-Strengthened CoNiFeMnCr HEAs at 1100 °C
by Patrice Berthod and Lionel Aranda
Micro 2024, 4(4), 751-764; https://doi.org/10.3390/micro4040046 - 3 Dec 2024
Viewed by 891
Abstract
The reinforcement of cast Cantor’s-type high-entropy alloys by MC carbides and their effect on the hot oxidation behavior were investigated. Three equimolar CoNiFeMnCr alloys without or with carbon and with either hafnium or tantalum were elaborated. Their as-cast microstructures were specified. Oxidation tests [...] Read more.
The reinforcement of cast Cantor’s-type high-entropy alloys by MC carbides and their effect on the hot oxidation behavior were investigated. Three equimolar CoNiFeMnCr alloys without or with carbon and with either hafnium or tantalum were elaborated. Their as-cast microstructures were specified. Oxidation tests were carried out in air at 1100 °C. Flexural creep tests were performed at 1100 °C at 10 MPa. The carbide-free CoNiFeMnCr alloy was single-phased. The version with Hf and C added and the one with Ta and C added contained interdendritic eutectic script HfC and TaC carbides, respectively. After oxidation for 50 h at 1100 °C, all alloys were covered by a (Cr,Mn)2O3 scale with various proportions of Cr and Mn. HfO2 or CrTaO4 also formed. Oxidation resulted in a deep depletion in Cr and in Mn in the subsurface. Oxidation is much faster for the three alloys by comparison with chromia-forming alloys. Their bad oxidation behavior is obviously due to Mn and protection by coating is to be considered. The creep deformation of the carbide-free CoNiFeMnCr alloy was very fast. The creep resistance of the two versions reinforced by either HfC or TaC deformed much slower. The addition of these MC carbides led to a deformation rate divided by five to ten times. Now, creep behavior comparisons with commercial alloys are to be conducted. They will be performed soon. Full article
(This article belongs to the Section Microscale Materials Science)
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