Advances in Micro- and Nanomaterials: Synthesis and Applications

A special issue of Micro (ISSN 2673-8023). This special issue belongs to the section "Microscale Materials Science".

Deadline for manuscript submissions: 31 December 2024 | Viewed by 11509

Special Issue Editor

Air Force Research Laboratory, Materials and Manufacturing Directorate, Dayton, OH 45433-7728, USA
Interests: nano materials; heterostructure; nanomaterials interface; nano materials design; modeling and simulation; nano and micro scale metrology
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Future materials are expected to perform in a disparate and dynamic environment with enhanced performance efficiency. In this pursuit, efficient materials often exhibit simultaneous multifunctionality (structural, electrical, thermal, optical, dielectric, etc.), even in very dynamic environments. Towards boosting materials performance or work efficiency, a compelling approach is to extract the same amount of work at every point of the materials volume, even in the gradient field. This may require placing different materials selectively at different locations (i.e., materials hybridization) to extract almost the same amount of work, whose effectiveness improves significantly if we can take such selectivity in a smaller (micron or atomic) scale—hence the importance of microscale or nanoscale materials science. Science-related materials selection and design at the micro- or nanoatomic scale materials hybridization (such as materials interface optimization and its validation) is still evolving and offers unprecedented opportunities in expanding the materials design and performance space.

In this Special Issue, we solicit foundational work in materials processing, innovative materials characterization techniques, metrology, and materials modeling approaches towards advancing micro- or nanoscale materials science. We invite original research work in the broad materials application space (structural, thermal, electrical, magnetic, dielectric, and more), discovering innovative micro- or nanoscale materials science issues.

Dr. Ajit Roy
Guest Editor

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Keywords

  • materials processing
  • innovative materials
  • micro- or nanoscale materials science
  • materials application
  • materials hybridization

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Published Papers (10 papers)

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Research

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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
Viewed by 402
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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13 pages, 3147 KiB  
Article
Photocatalytic Degradation of Methylene Blue by Surface-Modified SnO2/Se-Doped QDs
by Luis Alamo-Nole and Sonia J. Bailon-Ruiz
Micro 2024, 4(4), 721-733; https://doi.org/10.3390/micro4040044 - 21 Nov 2024
Viewed by 467
Abstract
Developing new nanomaterials and performing functionalization to increase their photocatalytic capacity are essential in developing low-cost, eco-friendly, and multipurpose-capacity catalysts. In this research, SnO2/Se-doped quantum dots (QDs) covered with glycerol (SnO2/Se-GLY) were synthesized using microwave irradiation. Then, their cover [...] Read more.
Developing new nanomaterials and performing functionalization to increase their photocatalytic capacity are essential in developing low-cost, eco-friendly, and multipurpose-capacity catalysts. In this research, SnO2/Se-doped quantum dots (QDs) covered with glycerol (SnO2/Se-GLY) were synthesized using microwave irradiation. Then, their cover was replaced with glutaraldehyde through a ligand exchange procedure (SnO2/Se-GLUT). The XRD analyses confirmed a tetragonal rutile structure of SnO2. The HR-TEM analysis confirmed the generation of QDs with a size around 8 nm, and the optical analysis evidenced low bandgap energies of 3.25 and 3.26 eV for the SnO2/Se-GLY and SnO2/Se-GLUT QDs, respectively. Zeta-sizer analysis showed that the hydrodynamic sizes for both nanoparticles were around 230 nm (50 mg/L), and the zeta potential confirmed that SnO2/Se-GLUT QDs were more stable than SnO2/Se-GLY QDs. The cover-modified QDs (SnO2/Se-GLUT) showed a higher and faster adsorption capacity, followed by a slower photocatalytic process than the original QDs (SnO2/Se-GLY). The QTOF-LC-MS analysis confirmed MB degradation through the identification of intermediates such as azure A, azure B, azure C, and phenothiazine. Adsorption isotherm analysis indicated Langmuir model compliance, supporting the high monolayer adsorption capacity and efficiency of these QDs as adsorbent/photocatalytic agents for organic pollutant removal. This dual capability for adsorption and photodegradation, along with the demonstrated reusability, highlights the potential of SnO2/Se QDs in wastewater treatment and environmental remediation. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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11 pages, 1886 KiB  
Article
Rapid Synthesis of Non-Toxic, Water-Stable Carbon Dots Using Microwave Irradiation
by Olga Soledad-Flores, Sonia J. Bailón-Ruiz and Félix Román-Velázquez
Micro 2024, 4(4), 659-669; https://doi.org/10.3390/micro4040040 - 9 Nov 2024
Viewed by 618
Abstract
Carbon dots (C-Dots) have garnered significant attention in various fields, including biomedical applications, photocatalysis, sensing, and optoelectronics, due to their high luminescence, biocompatibility, and ease of functionalization. However, concerns regarding their potential toxicity persist. Conventional synthesis methods for C-Dots often require long reaction [...] Read more.
Carbon dots (C-Dots) have garnered significant attention in various fields, including biomedical applications, photocatalysis, sensing, and optoelectronics, due to their high luminescence, biocompatibility, and ease of functionalization. However, concerns regarding their potential toxicity persist. Conventional synthesis methods for C-Dots often require long reaction times, high pressures, expensive equipment, extreme temperatures, and toxic reagents. In contrast, microwave irradiation provides a rapid, cost-effective, and scalable alternative for the synthesis of high-quality C-Dots. In this study, we report the single-step, 3-min synthesis of water-stable carbon dots at 100 °C, 120 °C, and 140 °C using microwave irradiation. Particle stability was achieved through polyethyleneimine (PEI) functionalization. The toxicity of the synthesized carbon dots was evaluated in marine crustaceans, revealing that C-Dots with an estimated size below 10 nm did not exhibit toxicity after 24 and 48 h of exposure. These findings demonstrate the potential of microwave-synthesized carbon dots as non-toxic, water-stable nanomaterials for environmental and biomedical applications. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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14 pages, 4863 KiB  
Article
Synthesis and Functionalities of Blade-Coated Nanographite Films
by Paloma E. S. Pellegrini, Luana de Moraes Leitão Gonçalves Vaz, Silvia Vaz Guerra Nista, Hugo Enrique Hernández-Figueroa and Stanislav Moshkalev
Micro 2024, 4(3), 460-473; https://doi.org/10.3390/micro4030029 - 27 Jul 2024
Viewed by 803
Abstract
The manufacturing and characterization of nanographite films on substrates form the foundation for advances in materials science. Conductive graphite films are challenging products, as isolating graphite oxide is often necessary. In this study, nanographite suspensions containing non-oxidized graphite flakes were used to fabricate [...] Read more.
The manufacturing and characterization of nanographite films on substrates form the foundation for advances in materials science. Conductive graphite films are challenging products, as isolating graphite oxide is often necessary. In this study, nanographite suspensions containing non-oxidized graphite flakes were used to fabricate novel thin and ultrathin films via blade coating on industry-standard substrates. Films as thin as 346 nm were successfully fabricated. Moreover, it was possible to induce the orientation of the graphite nanoflakes via blade coating. This orientation led to electrical anisotropy; thus, the electrical behavior of the films in each orthogonal direction differed. After adjusting the coating parameters and the concentration of the nanographite flakes, the electrical conductivity ranged from 0.04 S/cm to 0.33 S/cm. In addition, with such adjustments, the transparency of the films in the visible range varied from 20% to 75%. By establishing a methodology for the tuning of both electrical and optical properties via adjustments in the nanographite suspension and coating parameters, we can fabricate resistant, conductive, and transparent films satisfying certain requirements. The results presented here can be extrapolated to enhance applications, especially for photonics and solar cells, in fields that require electrical conductive materials with high levels of transparency. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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16 pages, 7273 KiB  
Article
Optical and Morphological Characterization of Nanoscale Oxides Grown in Low-Energy H+-Implanted c-Silicon
by Anna Szekeres, Sashka Alexandrova, Mihai Anastasescu, Hermine Stroescu, Mariuca Gartner and Peter Petrik
Micro 2024, 4(3), 426-441; https://doi.org/10.3390/micro4030027 - 18 Jul 2024
Viewed by 1055
Abstract
Nanoscale oxides grown in c-silicon, implanted with low-energy (2 keV) H+ ions and fluences ranging from 1013 cm−2 to 1015 cm−2 by RF plasma immersion implantation (PII), have been investigated. The oxidation of the implanted Si layers proceeded [...] Read more.
Nanoscale oxides grown in c-silicon, implanted with low-energy (2 keV) H+ ions and fluences ranging from 1013 cm−2 to 1015 cm−2 by RF plasma immersion implantation (PII), have been investigated. The oxidation of the implanted Si layers proceeded in dry O2 at temperatures of 700 °C, 750 °C and 800 °C. The optical characterization of the formed Si/SiOx structures was conducted by electroreflectance (ER) and spectroscopic ellipsometric (SE) measurements. From the ER and SE spectra analysis, the characteristic energy bands of direct electron transitions in Si are elaborated. The stress in dependence on hydrogenation conditions is considered and related to the energy shifts of the Si interband transitions around 3.4 eV. Silicon oxides, grown on PII Si at a low H+ fluence, have a non-stoichiometric nature, as revealed by IR-SE spectra analysis, while with an increasing H+ fluence in the PII Si substrates and/or the subsequent oxidation temperature the stoichiometric Si-O4 units in the oxides become predominant. The development of surface morphology is studied by atomic force microscopy (AFM) imaging. Oxidation of the H+-implanted Si surface region flattens out the surface pits created on the Si surface by H+ implants. Based on the evaluation of the texture index and mean fractal dimension, the isotropic and self-similar character of the studied surfaces is emphasized. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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11 pages, 5666 KiB  
Article
Preparation of Antimony Tin Oxide Thin Film Using Green Synthesized Nanoparticles by E-Beam Technique for NO2 Gas Sensing
by Chaitra Chandraiah, Hullekere Mahadevaiah Kalpana, Challaghatta Muniyappa Ananda and Madhusudan B. Kulkarni
Micro 2024, 4(3), 401-411; https://doi.org/10.3390/micro4030025 - 21 Jun 2024
Viewed by 1237
Abstract
This work delves into the preparation of ATO thin films and their characterization, fabrication, and calibration of a NO2 gas sensor, as well as the development of the packaged sensor. ATO thin films were prepared by e-beam evaporation using green synthesized ATO [...] Read more.
This work delves into the preparation of ATO thin films and their characterization, fabrication, and calibration of a NO2 gas sensor, as well as the development of the packaged sensor. ATO thin films were prepared by e-beam evaporation using green synthesized ATO nanomaterials on different substrates and annealed at 500 and 600 °C for one hour. The structural and morphological properties of the developed thin films were studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD) techniques. An orthorhombic SnO2 crystal structure was recognized through XRD analysis. The granular-shaped nanoparticles were revealed through SEM and TEM images. The films annealed at 600 °C exhibited improved crystallinity. ATO films prepared on normal 5 µm interdigitated electrodes (IDEs) and annealed at 600 °C exhibited a response of 10.31 ± 0.25 with an optimum temperature of 200 °C for a 4.8 ppm NO2 gas concentration. The packaged NO2 gas sensor developed using IDEs with a microheater demonstrated an improved response of 16.20 ± 0.25 for 4.8 ppm of NO2 gas. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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14 pages, 2381 KiB  
Article
Extending Polymer Opal Structural Color Properties into the Near-Infrared
by Giselle Rosetta, Matthew Gunn, John J. Tomes, Mike Butters and Chris E. Finlayson
Micro 2024, 4(2), 387-400; https://doi.org/10.3390/micro4020024 - 5 Jun 2024
Viewed by 1192
Abstract
We report the fabrication and characterisation of near-IR reflecting films and coatings based on shear-assembled crystalline ensembles of polymer composite microspheres, also known as “polymer opals”. Extension of the emulsion polymerisation techniques for synthesis of tractable larger core-interlayer-shell (CIS) particles, of up to [...] Read more.
We report the fabrication and characterisation of near-IR reflecting films and coatings based on shear-assembled crystalline ensembles of polymer composite microspheres, also known as “polymer opals”. Extension of the emulsion polymerisation techniques for synthesis of tractable larger core-interlayer-shell (CIS) particles, of up to half a micron diameter, facilitates the engineering and processing of thin-film synthetic opals, with a tunable photonic stopband spanning an extended spectral range of λ ≈ 700–1600 nm. Samples exhibit strong “scattering cone” interactions, with considerable angular dependence and angle tuning possible, as measured with a goniometric technique. These intense optical resonances in the near-IR, particularly within the important region around λ ~ 800 nm, combined with an appreciable translucency within the visible light spectrum, is indicative of the potential applications in coatings technologies and solar cells. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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15 pages, 6836 KiB  
Article
An Investigation into the Effect of Length Scale of Reinforcement on the Cryogenic Response of a Mg/2wt.%CeO2 Composite
by Shwetabh Gupta, Michael Johanes, Gururaj Parande and Manoj Gupta
Micro 2024, 4(1), 170-184; https://doi.org/10.3390/micro4010012 - 14 Mar 2024
Cited by 1 | Viewed by 999
Abstract
The present study attempted for the first time an investigation on the effect of deep cryogenic treatment in liquid nitrogen (LN) on magnesium–cerium oxide (Mg/2wt.%CeO2) composites containing equal amounts of different length scales (micron and nanosize) cerium oxide (CeO2) [...] Read more.
The present study attempted for the first time an investigation on the effect of deep cryogenic treatment in liquid nitrogen (LN) on magnesium–cerium oxide (Mg/2wt.%CeO2) composites containing equal amounts of different length scales (micron and nanosize) cerium oxide (CeO2) particles. The disintegrated melt deposition method was used to synthesize Mg-2CeO2 micro- and nanocomposites, followed by hot extrusion as the secondary processing. Further liquid nitrogen treatment was performed at a cryogenic temperature of −196 °C. The combined effects of cryogenic treatment and reinforcement length scale on physical, mechanical, and thermal behaviors were studied. The results indicate that LN-treated micro- and nanocomposite samples exhibit, in common, a reduction in porosity, similar grain size, and a limited effect on the original texture of the matrix. However, microhardness, 0.2% Compressive Yield Strength (CYS), failure strain, and energy absorbed increased for both micro- and nanocomposite samples. Overall, results clearly indicate the capability of deep cryogenic treatment with LN to positively diversify the properties of both micro- and nanocomposite samples. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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Review

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20 pages, 8642 KiB  
Review
Chemistry and Physics of Wet Foam Stability for Porous Ceramics: A Review
by Kamrun Nahar Fatema, Md Rokon Ud Dowla Biswas, Jung Gyu Park and Ik Jin Kim
Micro 2024, 4(4), 552-571; https://doi.org/10.3390/micro4040034 - 30 Sep 2024
Viewed by 971
Abstract
The unique structural properties of porous ceramics, such as low thermal conductivity, high surface area, controlled permeability, and low density, make this material valuable for a wide range of applications. Its uses include insulation, catalyst carriers, filters, bio-scaffolds for tissue engineering, and composite [...] Read more.
The unique structural properties of porous ceramics, such as low thermal conductivity, high surface area, controlled permeability, and low density, make this material valuable for a wide range of applications. Its uses include insulation, catalyst carriers, filters, bio-scaffolds for tissue engineering, and composite manufacturing. However, existing processing methods for porous ceramics, namely replica techniques and sacrificial templates, are complex, release harmful gases, have limited microstructure control, and are expensive. In contrast, the direct foaming method offers a simple and cost-effective approach. By modifying the surface chemistry of ceramic particles in a colloidal suspension, the hydrophilic particles are transformed into hydrophobic ones using surfactants. This method produces porous ceramics with interconnected pores, creating a hierarchical structure that is suitable for applications like nano-filters. This review emphasizes the importance of interconnected porosity in developing advanced ceramic materials with tailored properties for various applications. Interconnected pores play a vital role in facilitating mass transport, improving mechanical properties, and enabling fluid or gas infiltration. This level of porosity control allows for the customization of ceramic materials for specific purposes, including filtration, catalysis, energy storage, and biomaterials. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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52 pages, 6842 KiB  
Review
Porous Inorganic Nanomaterials: Their Evolution towards Hierarchical Porous Nanostructures
by Anitta Jose, Tom Mathew, Nora Fernández-Navas and Christine Joy Querebillo
Micro 2024, 4(2), 229-280; https://doi.org/10.3390/micro4020016 - 18 Apr 2024
Viewed by 2518
Abstract
The advancement of both porous materials and nanomaterials has brought about porous nanomaterials. These new materials present advantages both due to their porosity and nano-size: small size apt for micro/nano device integration or in vivo transport, large surface area for guest/target molecule adsorption [...] Read more.
The advancement of both porous materials and nanomaterials has brought about porous nanomaterials. These new materials present advantages both due to their porosity and nano-size: small size apt for micro/nano device integration or in vivo transport, large surface area for guest/target molecule adsorption and interaction, porous channels providing accessibility to active/surface sites, and exposed reactive surface/active sites induced by uncoordinated bonds. These properties prove useful for the development of different porous composition types (metal oxides, silica, zeolites, amorphous oxides, nanoarrays, precious metals, non-precious metals, MOFs, carbon nanostructures, MXenes, and others) through different synthetic procedures—templating, colloidal synthesis, hydrothermal approach, sol-gel route, self-assembly, dealloying, galvanostatic replacement, and so—for different applications, such as catalysis (water-splitting, etc.), biosensing, energy storage (batteries, supercapacitors), actuators, SERS, and bio applications. Here, these are presented according to different material types showing the evolution of the structure design and development towards the formation of hierarchical porous structures, emphasizing that the formation of porous nanostructures came about out of the desire and need to form hierarchical porous nanostructures. Common trends observed across these different composition types include similar (aforementioned) applications and the use of porous nanomaterials as templates/precursors to create novel ones. Towards the end, a discussion on the link between technological advancements and the development of porous nanomaterials paves the way to present future perspectives on these nanomaterials and their hierarchical porous architectures. Together with a summary, these are given in the conclusion. Full article
(This article belongs to the Special Issue Advances in Micro- and Nanomaterials: Synthesis and Applications)
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