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Keywords = microwave-assisted route

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32 pages, 4464 KiB  
Review
Multifunctional Polyimide for Packaging and Thermal Management of Electronics: Design, Synthesis, Molecular Structure, and Composite Engineering
by Xi Chen, Xin Fu, Zhansheng Chen, Zaiteng Zhai, Hongkang Miu and Peng Tao
Nanomaterials 2025, 15(15), 1148; https://doi.org/10.3390/nano15151148 - 24 Jul 2025
Viewed by 474
Abstract
Polyimide, a class of high-performance polymers, is renowned for its exceptional thermal stability, mechanical strength, and chemical resistance. However, in the context of high-integration and high-frequency electronic packaging, polyimides face critical challenges including relatively high dielectric constants, inadequate thermal conductivity, and mechanical brittleness. [...] Read more.
Polyimide, a class of high-performance polymers, is renowned for its exceptional thermal stability, mechanical strength, and chemical resistance. However, in the context of high-integration and high-frequency electronic packaging, polyimides face critical challenges including relatively high dielectric constants, inadequate thermal conductivity, and mechanical brittleness. Recent advances have focused on molecular design and composite engineering strategies to address these limitations. This review first summarizes the intrinsic properties of polyimides, followed by a systematic discussion of chemical synthesis, surface modification approaches, molecular design principles, and composite fabrication methods. We comprehensively examine both conventional polymerization synthetic routes and emerging techniques such as microwave-assisted thermal imidization and chemical vapor deposition. Special emphasis is placed on porous structure engineering via solid-template and liquid-template methods. Three key modification strategies are highlighted: (1) surface modifications for enhanced hydrophobicity, chemical stability, and tribological properties; (2) molecular design for optimized dielectric performance and thermal stability; and (3) composite engineering for developing high-thermal-conductivity materials with improved mechanical strength and electromagnetic interference (EMI) shielding capabilities. The dielectric constant of polyimide is reduced while chemical stability and wear resistance can be enhanced through the introduction of fluorine groups. Ultra-low dielectric constant and high-temperature resistance can be achieved by employing rigid monomers and porous structures. Furthermore, the incorporation of fillers such as graphene and boron nitride can endow the composite materials with high thermal conductivity, excellent EMI shielding efficiency, and improved mechanical properties. Finally, we discuss representative applications of polyimide and composites in electronic device packaging, EMI shielding, and thermal management systems, providing insights into future development directions. Full article
(This article belongs to the Special Issue Functional and Structural Properties of Polymeric Nanocomposites)
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26 pages, 5399 KiB  
Article
Microwave-Assisted Pyrolysis of Polyethylene and Polypropylene from End-of-Life Vehicles: Hydrogen Production and Energy Valorization
by Grigore Psenovschi, Ioan Calinescu, Alexandru Fiti, Ciprian-Gabriel Chisega-Negrila, Sorin-Lucian Ionascu and Lucica Barbes
Sustainability 2025, 17(13), 6196; https://doi.org/10.3390/su17136196 - 6 Jul 2025
Viewed by 632
Abstract
Plastic waste is currently a major concern in Romania due to the annual increase in quantities generated from anthropogenic and industrial activities, especially from end-of-life vehicles (ELVs), and the need to reduce environmental impact. This study investigates an alternative valorization route for polypropylene [...] Read more.
Plastic waste is currently a major concern in Romania due to the annual increase in quantities generated from anthropogenic and industrial activities, especially from end-of-life vehicles (ELVs), and the need to reduce environmental impact. This study investigates an alternative valorization route for polypropylene (PP) and polyethylene (PE) plastic waste through microwave-assisted pyrolysis, aiming to maximize conversion into gaseous products, particularly hydrogen-rich gas. A monomode microwave reactor was employed, using layered configurations of plastic feedstock, silicon carbide as a microwave susceptor, and activated carbon as a catalyst. The influence of catalyst loading, reactor configuration, and plastic type was assessed through systematic experiments. Results showed that technical-grade PP, under optimal conditions, yielded up to 81.4 wt.% gas with a hydrogen concentration of 45.2 vol.% and a hydrogen efficiency of 44.8 g/g. In contrast, PE and mixed PP + PE waste displayed lower hydrogen performance, particularly when containing inorganic fillers. For all types of plastics studied, the gaseous fractions obtained have a high calorific value (46,941–55,087 kJ/kg) and at the same time low specific CO2 emissions (4.4–6.1 × 10−5 kg CO2/kJ), which makes these fuels very efficient and have a low carbon footprint. Comparative tests using conventional heating revealed significantly lower hydrogen yields (4.77 vs. 19.7 mmol/g plastic). These findings highlight the potential of microwave-assisted pyrolysis as an efficient method for transforming ELV-derived plastic waste into energy carriers, offering a pathway toward low-carbon, resource-efficient waste management. Full article
(This article belongs to the Special Issue Novel and Scalable Technologies for Sustainable Waste Management)
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17 pages, 1570 KiB  
Article
Overcoming Scaling Challenges in Sol–Gel Synthesis: A Microwave-Assisted Approach for Iron-Based Energy Materials
by Judith González-Lavín, Ana Arenillas and Natalia Rey-Raap
Microwave 2025, 1(2), 6; https://doi.org/10.3390/microwave1020006 - 30 Jun 2025
Viewed by 315
Abstract
There is currently an effort to scale up sol–gel nanomaterials without compromising quality, and microwave heating can pave the way for this due to its heating efficiency, resulting in a fast and homogeneous process. In this work, the sol–gel synthesis of transition metal [...] Read more.
There is currently an effort to scale up sol–gel nanomaterials without compromising quality, and microwave heating can pave the way for this due to its heating efficiency, resulting in a fast and homogeneous process. In this work, the sol–gel synthesis of transition metal aerogels, specifically iron-based aerogels, is studied using a microwave-assisted sol–gel methodology in an open-system multimode device as a potential route to scale-up production. Different approaches were tested to evaluate the best way to increase yield per batch, with different vessel shapes and volumes. It is shown that the shape and size of the vessel can be determinant in the interaction with microwaves and, thus, in the heating process, influencing the sol–gel reactions and the characteristics and homogeneity of the obtained nanomaterials. It has been found that a wide vessel is preferable to a tall and narrow one since the heating process is more homogeneous in the former and the sol–gel and cross-linking reactions take place earlier, which improves the mechanical properties of the final nanomaterial. For mass production of nanomaterials, the interaction of the reagents with the microwave field must be considered, and this depends not only on their nature but also on their volume, shape, and arrangement inside the cavity. Full article
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12 pages, 2545 KiB  
Article
Rapid Fabrication of ZSM-5/AlPO4-5 Composites via Microwave-Ionothermal Strategy for Enhanced Methanol-to-Olefins Catalysis
by Li Han, Mengting Zhang, Hao Li, Huiru Ding, Jingjing Zhao, Yujia Zhang, Lang Wu, Changzhou Jiao, Jie Feng and Zhikun Peng
Catalysts 2025, 15(6), 605; https://doi.org/10.3390/catal15060605 - 19 Jun 2025
Viewed by 503
Abstract
Microwave-assisted ionothermal strategies offer an effective pathway for rapid zeolite crystallization under mild conditions, while conventional ionothermal approaches are still constrained by prolonged crystallization cycles that limit their industrial applicability. Herein, we report a microwave-activated, ionic liquid-mediated synthesis strategy that enables the precise [...] Read more.
Microwave-assisted ionothermal strategies offer an effective pathway for rapid zeolite crystallization under mild conditions, while conventional ionothermal approaches are still constrained by prolonged crystallization cycles that limit their industrial applicability. Herein, we report a microwave-activated, ionic liquid-mediated synthesis strategy that enables the precise modulation of crystallization kinetics and composite assembly. By introducing ZSM-5 seeds into the ionic liquid system, the nucleation and growth of AlPO4-5 were significantly accelerated, reducing crystallization time by up to 75% (optimal condition: 60 min). Among various imidazolium-based ionic liquids, [BMMIm]Br demonstrated an optimal balance of hydrophilic and hydrophobic interactions, yielding composite zeolites with high surface area (350 m2·g−1) and large pore volume (0.28 cm3·g−1). Comprehensive characterization (XRD, SEM-EDX, NH3-TPD) confirmed the formation of well-defined ZSM-5/AlPO4-5 core–shell structures and revealed tunable acid site distributions depending on the ionic liquid used. In methanol to olefins (MTO) reactions, the composite catalyst exhibited outstanding selectivity towards light olefins (C2=–C4=: 72.84%), markedly outperforming the individual ZSM-5 and AlPO4-5 components. The superior catalytic behavior is primarily attributed to the synergistic effect of hierarchical acid site tuning and the integrated core–shell architecture, which together optimize reaction selectivity. This strategy provides a promising route for the rational design of high-performance zeolites with significant industrial applicability. Full article
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26 pages, 2781 KiB  
Article
Pyrolysis Mechanism of Victorian Brown Coal Under Microwave and Conventional Conditions for Hydrogen-Rich Gas Production
by Quan Sun, Salman Khoshk Rish, Jianglong Yu and Arash Tahmasebi
Energies 2025, 18(11), 2863; https://doi.org/10.3390/en18112863 - 30 May 2025
Viewed by 462
Abstract
Fast microwave pyrolysis technology can effectively convert brown coal into hydrogen-rich syngas. However, the unique pyrolysis behaviour of brown coal under microwave conditions is not fully understood in comparison with conventional pyrolysis. This study used Victorian brown coal as a raw material to [...] Read more.
Fast microwave pyrolysis technology can effectively convert brown coal into hydrogen-rich syngas. However, the unique pyrolysis behaviour of brown coal under microwave conditions is not fully understood in comparison with conventional pyrolysis. This study used Victorian brown coal as a raw material to conduct pyrolysis experiments under conventional and microwave heating methods. The results demonstrate that the microwave-assisted pyrolysis of Victorian brown coal can selectively crack polar functional groups, enhancing H2 and CO production via radical-driven secondary reactions and gasification, while conventional heating favours the formation of tar containing phenols and fewer aromatic compounds. The result is a high-quality syngas (75.03 vol.%) with a hydrogen yield of 10.28 (mmol Gas/g Coal (daf)) at 700 °C under microwave heating, offering a scalable route for valorising low-rank coals. Full article
(This article belongs to the Special Issue Clean Utilization and Conversion Technologies of Coal)
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25 pages, 3654 KiB  
Review
Plasma-Assisted Hydrogen Production: Technologies, Challenges, and Future Prospects
by Lijian Wang, Xiaowei Guo, Jianzheng Liu, Chao Wang, Yi Wang, Yi Qiu, Zhongqian Ling, Xianyang Zeng and Dingkun Yuan
Processes 2025, 13(4), 1157; https://doi.org/10.3390/pr13041157 - 11 Apr 2025
Cited by 2 | Viewed by 2341
Abstract
As global demand for clean energy continues to rise, hydrogen, as an ideal energy carrier, plays a crucial role in the energy transition. Traditional hydrogen production methods predominantly rely on fossil fuels, leading to environmental pollution and energy inefficiency. In contrast, plasma-assisted hydrogen [...] Read more.
As global demand for clean energy continues to rise, hydrogen, as an ideal energy carrier, plays a crucial role in the energy transition. Traditional hydrogen production methods predominantly rely on fossil fuels, leading to environmental pollution and energy inefficiency. In contrast, plasma-assisted hydrogen production, as an emerging technology, has gained significant attention due to its high efficiency, environmental friendliness, and flexibility. Plasma technology generates high-energy electrons or ions by exciting gas molecules, which, under specific conditions, effectively decompose water vapor or hydrocarbon gases to produce hydrogen. This review systematically summarizes the basic principles, technological routes, research progress, and potential applications of plasma-assisted hydrogen production. It focuses on various plasma-based hydrogen production methods, such as water vapor decomposition, hydrocarbon cracking, arc discharge, and microwave discharge, highlighting their advantages and challenges. Additionally, it addresses key issues facing plasma-assisted hydrogen production, including energy efficiency improvement, reactor stability, and cost optimization, and discusses the future prospects of these technologies. With ongoing advancements, plasma-assisted hydrogen production is expected to become a mainstream technology for hydrogen production, contributing to global goals of zero carbon emissions and sustainable energy development. Full article
(This article belongs to the Section Chemical Processes and Systems)
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29 pages, 1891 KiB  
Article
Synthesis of Fluorinated Glycotope Mimetics Derived from Streptococcus pneumoniae Serotype 8 CPS
by Daniel Gast, Sebastian Neidig, Maximilian Reindl and Anja Hoffmann-Röder
Int. J. Mol. Sci. 2025, 26(4), 1535; https://doi.org/10.3390/ijms26041535 - 12 Feb 2025
Viewed by 1439
Abstract
Fluorination of carbohydrates is a promising strategy to produce glycomimetics with improved pharmacological properties, such as increased metabolic stability, bioavailability and protein-binding affinity. Fluoroglycans are not only of interest as inhibitors and chemical probes but are increasingly being used to develop potential synthetic [...] Read more.
Fluorination of carbohydrates is a promising strategy to produce glycomimetics with improved pharmacological properties, such as increased metabolic stability, bioavailability and protein-binding affinity. Fluoroglycans are not only of interest as inhibitors and chemical probes but are increasingly being used to develop potential synthetic vaccine candidates for cancer, HIV and bacterial infections. Despite their attractiveness, the synthesis of fluorinated oligosaccharides is still challenging, emphasizing the need for efficient protocols that allow for the site-specific incorporation of fluorine atoms (especially at late stages of the synthesis). This is particularly true for the development of fully synthetic vaccine candidates, whose (modified) carbohydrate antigen structures (glycotopes) per se comprise multistep synthesis routes. Based on a known minimal protective epitope from the capsular polysaccharide of S. pneumoniae serotype 8, a panel of six novel F-glycotope mimetics was synthesized, equipped with amine linkers for subsequent conjugation to immunogens. Next to the stepwise assembly via fluorinated building blocks, the corresponding 6F-substituted derivatives could be obtained by microwave-assisted, nucleophilic late-stage fluorination of tri- and tetrasaccharidic precursors in high yields. The described synthetic strategy allowed for preparation of the targeted fluorinated oligosaccharides in sufficient quantities for future immunological studies. Full article
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15 pages, 2591 KiB  
Article
Microwave-Assisted Reduction of Graphene Oxide to Reduced Graphene Oxide
by Jessica T. Mhlongo, Boitumelo Tlhaole, Linda Z. Linganiso, Tshwafo E. Motaung and Ella C. Linganiso-Dziike
Processes 2025, 13(1), 216; https://doi.org/10.3390/pr13010216 - 14 Jan 2025
Cited by 2 | Viewed by 1451
Abstract
Green chemistry seeks to find alternative synthesis routes that are less harsh to living organisms and the environment. In this communication, a microwave-assisted hydrothermal technique and a thermal annealing method were used in the reduction of graphene oxide (GO) to make reduced GO [...] Read more.
Green chemistry seeks to find alternative synthesis routes that are less harsh to living organisms and the environment. In this communication, a microwave-assisted hydrothermal technique and a thermal annealing method were used in the reduction of graphene oxide (GO) to make reduced GO (rGO). Graphite powder was oxidised using the Improved Hummers’ method, exfoliated, and freeze-dried. Thereafter, an aqueous suspension of GO was reduced under microwave (MW) irradiation for 10 min at 600 W with and without the help of a reducing agent (hydrazine hydrate). Thermal annealing reduction was also conducted under a nitrogen atmosphere at 300 °C for 1 h. Prepared samples were analysed using Raman laser spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), the Brunauer–Emmett–Teller (BET) method, and X-ray photoelectron spectroscopy (XPS). A successful reduction in the GO functional groups between the sheets was established using XRD. In the Raman analysis, the ratio of the intensity of the D and G band (ID/IG) in graphene sheets assisted in assessing the quality of the graphene films. An estimation of the number of structural defects was calculated using the ID/IG ratio. The Raman analysis showed an increase in the ID/IG ratio after both oxidation and reduction processes. The defect densities of both MW-treated samples were comparable while an increased defect density was evident in the thermally annealed sample. TEM micrographs confirmed the sheet-like morphology of the samples. The rGO sheets obtained from the MW-treated method appeared to be smaller when compared to the rGO ones obtained by thermal treatment. It was also evident from XRD analysis that thermal treatment promoted the coalition of graphitic layers, such that the estimated number of layers was larger than that of GO. The elemental analysis showed that the C/O ratio of GO increased from 2 to 7.8 after MW hydrazine reduction. Full article
(This article belongs to the Special Issue Microwave Conversion Technique Intensification, 2nd Edition)
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25 pages, 1711 KiB  
Review
Bimetallic and Trimetallic Catalysts Advancements in the Conventional and MW-Assisted Propane Dehydrogenation Process
by Olga Muccioli, Concetta Ruocco and Vincenzo Palma
Catalysts 2024, 14(12), 950; https://doi.org/10.3390/catal14120950 - 22 Dec 2024
Cited by 3 | Viewed by 1899
Abstract
A huge variety of chemical commodities are built from propylene molecules, and its conventional production technologies (naphtha steam cracking and fluid catalytic cracking) are unable to satisfy C3H6’s increasing requirements. In this scenario, Direct Propane Dehydrogenation (PDH) provides a [...] Read more.
A huge variety of chemical commodities are built from propylene molecules, and its conventional production technologies (naphtha steam cracking and fluid catalytic cracking) are unable to satisfy C3H6’s increasing requirements. In this scenario, Direct Propane Dehydrogenation (PDH) provides a practical and reliable route for supplying this short demand due to the economic availability of the raw material (C3H8) and the high propylene selectivities. The main challenges of propane dehydrogenation technology are related to the design of very active catalysts with negligible byproduct formation. In particular, the issue of catalyst deactivation by coke deposition still requires further development. In addition, PDH is a considerable endothermic reaction, and the efficiency of this technology is strictly related to heat transfer management. Thus, this current review specifically discusses the recent advances in highly dispersed bimetallic and trimetallic catalysts proposed for the PDH reaction in both conventional-heated and microwave-heated reactors. From the point of view of catalyst development, the recent research is mainly addressed to obtain nanometric and single-atom catalysts and core–shell alloys: atomically dispersed metal atoms promote the desorption of surface-bonded propylene and inhibit its further dehydrogenation. The discussion is focused on the alternative formulations proposed in the last few years, employing active species and supports different from the classical Pt-Sn/Al2O3 catalyst. Concerning the conventional route of energy-supply to the catalytic bed, the advantage of using a membrane as well as fluidized bed reactors is highlighted. Recent developments in alternative microwave-assisted dehydrogenation (PDH) employing innovative catalytic systems based on silicon carbide (SiC) facilitate selective heating of the catalyst. This advancement leads to improved catalytic activity and propylene selectivity while effectively reducing coke formation. Additionally, it promotes environmental sustainability in the ongoing electrification of chemical processes. Full article
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19 pages, 3489 KiB  
Article
Sustainable Valorization of Oil and Gas Industry Biosolids: Optimal Reuse Pathways
by Hesan Elfaki, Nivinya Hemachandra, Georg Stockinger, Ali Al-Sharshani, Sabah Solim and Dhabia M. Al-Mohannadi
Sustainability 2024, 16(22), 9738; https://doi.org/10.3390/su16229738 - 8 Nov 2024
Cited by 1 | Viewed by 1256
Abstract
This study investigates the potential of converting waste biosolids from industrial sources, focusing on economic viability and heavy metal removal efficiency. Traditional management methods like landfilling and incineration are increasingly impractical due to land constraints and environmental concerns, prompting a shift towards thermal [...] Read more.
This study investigates the potential of converting waste biosolids from industrial sources, focusing on economic viability and heavy metal removal efficiency. Traditional management methods like landfilling and incineration are increasingly impractical due to land constraints and environmental concerns, prompting a shift towards thermal and biological conversion technologies including anaerobic digestion, pyrolysis, gasification, and hydrothermal liquefaction. Incorporating a pretreatment for heavy metal removal is essential, as industrial wastes are highly subjected to metal contamination. The study screens a range of metal removal processes, including precipitation, adsorption, ion exchange, and microwave induction. Although a techno-economic analysis can help give a perspective on the economic viability and environmental impact of each technology, it does not account for technical limitations and variations in the treated waste stream. A mixed integer linear programming (MILP) optimization model is developed to fill in this gap and assist in waste stream allocation to the most appropriate technology, taking into account both technology capacities and feed characteristics. This study looked into the optimal treatment route at different feed moisture contents and varying flow rates. The results demonstrate that the model distributes the feed across the different technologies on the basis of maximizing the capacity of the optimal technology while ensuring the moisture and heavy metal content limits are satisfied. Thus, it maximizes profitability and ensures heavy metal removal efficiency. By optimizing industrial biosolids treatment pathways, this study promotes sustainable resource recovery aligning with circular economy principles in waste management. The developed model facilitates informed decision-making in biosolids management and industrial waste treatment practices. Full article
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10 pages, 2078 KiB  
Article
Microwave-Assisted Oxidation of N2 into NOx over a La-Ce-Mn-O Perovskite Yielding Plasmas in a Quartz Flow Reactor at Atmospheric Pressure
by Frederic C. Meunier and Akim Kaddouri
Catalysts 2024, 14(9), 635; https://doi.org/10.3390/catal14090635 - 19 Sep 2024
Cited by 1 | Viewed by 1462
Abstract
N2 oxidation to NOx is a challenging reaction, and alternative routes to the industrial Ostwald process are of interest. A perovskite under flowing O2-N2 mixtures at atmospheric pressure in a quartz tube reactor was irradiated by microwaves (MW), [...] Read more.
N2 oxidation to NOx is a challenging reaction, and alternative routes to the industrial Ostwald process are of interest. A perovskite under flowing O2-N2 mixtures at atmospheric pressure in a quartz tube reactor was irradiated by microwaves (MW), leading to the formation of hot spots and plasmas within the catalyst bed. NOx concentrations up to 2.5 vol.% in one pass were obtained at 600 W. Using a lower MW power of 100 W led to a pulsed mode yielding lower NOx concentrations and no noticeable damage to the quartz reactor. The formation of plasma was strongly dependent on the perovskite bed packing. The perovskite acted primarily as a susceptor and likely also as a catalyst, although the proportion of heterogeneous and homogenous reactions could not be determined in the present study. The simple reactor layout allowing operation at atmospheric pressure is promising for the development of practical MW-assisted N2 fixation technologies. Full article
(This article belongs to the Section Catalysis for Sustainable Energy)
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25 pages, 3064 KiB  
Review
The Catalytic Potential of Modified Clays: A Review
by Altantuya Ochirkhuyag and Jadambaa Temuujin
Minerals 2024, 14(6), 629; https://doi.org/10.3390/min14060629 - 20 Jun 2024
Cited by 8 | Viewed by 4068
Abstract
The need for innovative catalysts and catalytic support materials is continually growing due to demanding requirements, stricter environmental demands, and the ongoing development of new chemical processes. Since about 80% of all industrial processes involve catalysts, there is a continuing need to develop [...] Read more.
The need for innovative catalysts and catalytic support materials is continually growing due to demanding requirements, stricter environmental demands, and the ongoing development of new chemical processes. Since about 80% of all industrial processes involve catalysts, there is a continuing need to develop new catalyst materials and supports with suitable qualities to meet ongoing industrial demands. Not only must new catalysts have tailored properties, but they must also be suitable for large-scale production through environmentally friendly and cost-effective processes. Clay minerals, with their rich history in medicine and ceramics, are now emerging as potential catalysts. Their transformative potential is exemplified in applications such as hydrogenating the greenhouse gas CO2 into carbohydrate fuel, a crucial step in meeting the rising electrical demand. Moreover, advanced materials derived from clay minerals are proving their mettle in diverse photocatalytic reactions, from organic dye removal to pharmaceutical pollutant elimination and photocatalytic energy conversion through water splitting. Clay minerals in their natural state show a low catalytic activity, so to increase their reactivity, they must be activated. Depending on the requirements of a particular application, selecting an appropriate activation method for modifying a natural clay mineral is a critical consideration. Traditional clay mineral processing methods such as acid or alkaline treatment are used. Still, these have drawbacks such as high costs, long processing times, and the formation of hazardous by-products. Other activation processes, such as ultrasonication and mechanical activation routes, have been proposed to reduce the production of hazardous by-products. The main advantage of ultrasonication and microwave-assisted procedures is that they save time, whereas mechanochemical processing is simple and efficient. This short review focuses on modifying clay minerals using various new methods to create sophisticated and innovative new materials. Recent advances in catalytic reactions are specifically covered, including organic biogeochemical processes, photocatalytic processes, carbon nanotube synthesis, and energy conversion processes such as CO2 hydrogenation and dry reforming of methane. Full article
(This article belongs to the Section Clays and Engineered Mineral Materials)
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14 pages, 5391 KiB  
Article
The Role of Zn Ions in the Structural, Surface, and Gas-Sensing Properties of SnO2:Zn Nanocrystals Synthesized via a Microwave-Assisted Route
by Luís F. da Silva, Mattia A. Lucchini, Ariadne C. Catto, Waldir Avansi Jr., Sandrine Bernardini, Khalifa Aguir, Markus Niederberger and Elson Longo
Sensors 2024, 24(1), 140; https://doi.org/10.3390/s24010140 - 26 Dec 2023
Cited by 4 | Viewed by 1803
Abstract
Although semiconducting metal oxide (SMOx) nanoparticles (NPs) have attracted attention as sensing materials, the methodologies available to synthesize them with desirable properties are quite limited and/or often require relatively high energy consumption. Thus, we report herein the processing of Zn-doped SnO2 NPs [...] Read more.
Although semiconducting metal oxide (SMOx) nanoparticles (NPs) have attracted attention as sensing materials, the methodologies available to synthesize them with desirable properties are quite limited and/or often require relatively high energy consumption. Thus, we report herein the processing of Zn-doped SnO2 NPs via a microwave-assisted nonaqueous route at a relatively low temperature (160 °C) and with a short treatment time (20 min). In addition, the effects of adding Zn in the structural, electronic, and gas-sensing properties of SnO2 NPs were investigated. X-ray diffraction and high-resolution transmission electron microscopy analyses revealed the single-phase of rutile SnO2, with an average crystal size of 7 nm. X-ray absorption near edge spectroscopy measurements revealed the homogenous incorporation of Zn ions into the SnO2 network. Gas sensing tests showed that Zn-doped SnO2 NPs were highly sensitive to sub-ppm levels of NO2 gas at 150 °C, with good recovery and stability even under ambient moisture. We observed an increase in the response of the Zn-doped sample of up to 100 times compared to the pristine one. This enhancement in the gas-sensing performance was linked to the Zn ions that provided more surface oxygen defects acting as active sites for the NO2 adsorption on the sensing material. Full article
(This article belongs to the Special Issue Chemical Sensors—Recent Advances and Future Challenges 2023–2024)
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19 pages, 4056 KiB  
Article
Structural Transition in the Growth of Copper Terephthalate Metal–Organic Frameworks: Understanding the Effect of the Synthetic Protocol and Its Impact on Electrochemical Behavior
by Sara L. Rodríguez, Gabriela A. Ortega-Moreno, Manuel Sánchez-Sánchez, José L. Fernández and Juan M. Zamaro
Coatings 2023, 13(12), 2065; https://doi.org/10.3390/coatings13122065 - 10 Dec 2023
Cited by 3 | Viewed by 2764
Abstract
Some copper-based metal–organic frameworks show promise for use as electrocatalysts because they allow for an electrode configuration in which copper species with redox and electron-conducting properties are immobilized in a three-dimensional arrangement. This work shows that the synthesis of copper terephthalates (Cu-BDCs) can [...] Read more.
Some copper-based metal–organic frameworks show promise for use as electrocatalysts because they allow for an electrode configuration in which copper species with redox and electron-conducting properties are immobilized in a three-dimensional arrangement. This work shows that the synthesis of copper terephthalates (Cu-BDCs) can lead to rigid structures of the copper hydroxyterephthalate-type or flexible structures that are isoreticular to the MOF-2 type, depending solely on the synthesis route. Here, a detailed analysis of the syntheses of the crystals is carried out employing protocols with different solvents as well as conventional or microwave-assisted solvothermal methods. All solids were fully characterized by a combination of characterization techniques, such as FE-SEM, T-XRD, TGA, and FTIR, and their electrochemical redox responses were also evaluated by cyclic voltammetry. A correlation between the Cu-BDCs structures and their electrochemical behaviors was established and a new version of an electroactive copper hydroxyterephthalate was synthesized by a microwave method in 3 h with a dimethylformamide-free protocol. This Cu-BDC was obtained as dispersed nanoflakes with a high amount of copper sites and the capacity to be reversibly electroreduced-oxidized and showed catalytic activity in the oxygen reduction reaction (ORR). Full article
(This article belongs to the Special Issue Advanced Research on Energy Storage Materials and Devices)
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14 pages, 9198 KiB  
Article
Study of the Synthesis Variables in the Preparation of CoAl2O4 Pigment Using Microwaves to Reduce Energetic Consumption
by Guillermo Paulo-Redondo and Isaac Nebot-Díaz
Eng 2023, 4(4), 2826-2839; https://doi.org/10.3390/eng4040159 - 14 Nov 2023
Cited by 2 | Viewed by 1270
Abstract
Due to the importance of optimizing the manufacture of ceramic pigments, motivated by the increase in prices of both raw materials and energy, and the need to control manufacturing parameters to obtain optimal conditions for the preparation of ceramic inks, two synthesis routes [...] Read more.
Due to the importance of optimizing the manufacture of ceramic pigments, motivated by the increase in prices of both raw materials and energy, and the need to control manufacturing parameters to obtain optimal conditions for the preparation of ceramic inks, two synthesis routes (traditional route and coprecipitation) and two calcination methods (traditional oven and microwave oven) are proposed to obtain the blue ceramic pigment CoAl2O4 with the aim of minimizing the use of mineralizers or flux agents and reducing energy consumption in its manufacturing. The pigments prepared were characterized by thermal analysis and structurally by XRD and SEM, with particle sizes below 300 nm observed. Finally, the colorimetric coordinates of glazed tiles with the pigments obtained were characterized. In all cases, the microwave-assisted synthesis increased the color intensity, considerably decreasing the temperature and calcination time, obtaining a particle size under 300 nm with a very narrow size distribution, and substantially improving the energy cost of its preparation and the color development of the final product. The viability of the combination of synthesis by coprecipitation and microwave calcination as a method of industrial preparation of ceramic pigments has been demonstrated. Full article
(This article belongs to the Section Materials Engineering)
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