Method For Synthesis Research Articles

Eco-Friendly Synthesis of Amino and Carboxyl-Functionalized Silica Nanoparticles for Enhanced Adsorption of Water Pollutants

Green synthesized nanoparticles (NPs) have garnered significant attention as a rapidly expanding category of materials with diverse applications. In this context, plants are widely acknowledged as a highly favourable option for green synthesis due to their adherence to the eco-friendly pathway of NPs biosynthesis. The objective of green synthesis is to reduce the utilisation of hazardous chemicals. The utilisation of silica (SiO2) NPs, synthesised from biomass as adsorbents, has shown great potential particularly in removing toxic materials from environment. When it comes to adsorbing water pollutants, functionalized SiO2 NPs are seen as potential option. However, certain functional group onto the surface of SiO2 NPs have higher affinity towards a particular pollutant. In this work, a simple and eco-friendly synthesis method (using waste bamboo leaves) have been utilized for production of SiO2 NPs. Further, a silylating procedure was used to functionalize SiO2 NPs with amine (A-SiO2) and carboxyl groups (C-SiO2) for determining adsorption capabilities towards anionic and cationic dyes i.e., Naphthol green-B and brilliant green. The adsorption mechanism has been discussed in view of different adsorption isotherm models. According to batch investigations, the functionalized SiO2 NPs showed different behaviour for dyes depending upon nature of dyes and the functional groups. The results of the study revealed that A-SiO2 NPs were having adsorption capacity of 122.10 mg/g for anionic dye (NGB) while C-SiO2 NPs showed adsorption capacity of 114.41 mg/g for cationic dye (BG). Additionally, these NPs exhibit good recyclability up to 5 cycles of reuse. Novelty of this study is the reduced energy needs for the green synthesis of the SiO2 NPs using bamboo leaves and the effect of different functional groups on the adsorption capacity of the NPs. Overall, this study provides a sustainable, and reusable approach for effective dye removal from wastewater, addressing both environmental and economic problems.

Facile one-pot fabrication of multifunctional silver nanoparticles utilizing biowaste for efficient pollutant degradation, heavy metal sensing, and bactericidal activity

Citrus peels constitute around 8-10% of total fruit biomass and are an abundant source of functional organic compounds, however, they are commonly regarded as waste and discarded. This study presents a facile one-pot synthesis method for the fabrication of multifunctional silver nanoparticles using the biowaste as a reducing, capping, and stabilizing agent for the synthesis. The utilization of biowaste not only aligns with sustainable practices but also imparts unique characteristics to the nanoparticles for diverse functionalities. Extensive spectroscopic and microscopic characterization validate the stability of the resulting AgNPs with an average diameter of 40nm. The synthesized nanoparticles exhibit enhanced catalytic activities for complete degradation of toxic nitroaromatic pollutant 4-nitrophenol within 21 min. Additionally, the sensing capabilities of AgNPs render them highly sensitive to heavy metal mercury, offering potential applications in environmental monitoring. Furthermore, the AgNPs demonstrate comprehensive bactericidal properties tested against S. aureus at 0.0625 mg/mL, highlighting their potential in biomedical applications. Moreover, density-functional theory (DFT) studies were performed to compare the reducing and stabilizing characteristics of the main components present in the fruit peel extract, with ferulic acid identified as theoretically the most potent compound. This research introduces a promising avenue for the development of versatile nanoparticles with multifaceted properties utilizing the potential of biowaste to address crucial challenges in environmental remediation.

Graphene-based photocatalytic membrane application for the remediation of organic dye pollutants: A review

The inadequate elimination of emerging organic contaminants, such as pharmaceuticals and personal care items, presents a substantial risk to water security in treating wastewater and its subsequent discharge into the receiving water bodies or recharging ground water. A practical solution can be found by combining hybrid photocatalytic oxidation with membrane separation technologies. The review examines the crucial process of strengthening photocatalytic membranes by including graphene and its derivatives. Further, it highlights the graphene’s ability to improve anti-fouling properties with increased efficiency of pollutant degradation. An in-depth analysis of the synthesis method and its impact on graphene-based photocatalytic membranes' morphology and photocatalytic characteristics is conducted. In addition to discussing membrane alteration, the review delves into the different elements and complexities involved in optimising filtration performance. Adding a comparison with carbon-based support membranes enhances the overall understating of graphene's importance in the membrane matrix. Economic and life cycle aspects have also been elaborated to gauge the practical viability of these neoteric photoactive membranes. The present article also pinpoints the existing lacuna and lays forward potential solutions that can assist in broader acceptance of these membrane for contaminant remediation. Though development of graphene-based photocatalytic membranes is still in embryonic phase, the review advocates it as a sustainable successor to conventional membrane-based treatment in the future.

Value addition of MXenes as photo-/electrocatalysts in water splitting for sustainable hydrogen production.

The energy transition from fossil fuel-based to renewable energy is a global agenda. At present, a major concern in the green hydrogen economy is the demand for clean fuels and non-noble materials to produce hydrogen through water splitting. Researchers are focusing on addressing this concern with the help of the development of appropriate non-noble-based photo-/electrocatalytic materials. A new class of two-dimensional materials, MXenes, have recently shown tremendous potential for water splitting to produce H2via a photoelectrochemical process. The unique properties of emerging 2D MXene materials, such as hydrophilic surface functionalities, higher surface-to-volume ratios, and inherent flexibility, present these materials as appropriate photo-/electrocatalytic materials. Unique value addition and innovative strategies such as the introduction of end-group modification, heterojunctions, and nanostructure engineering have shown the potential of MXene materials as emerging photo-/electrocatalysts for water splitting. When integrated with conventional noble metal catalysts, MXene-based catalysts demonstrated a lower overpotential for hydrogen and oxygen evolution reactions and a remarkable boost in performance for enhanced H2 production rates surpassing those of pristine noble metal-based catalysts. These promote future perspectives for the utilization of chemically synthesized MXenes as alternative photo-/electrocatalysts. Future research direction should focus on MXene synthesis and utilization for surface modification, composite formation, stabilization, and optimization in synthesis methods and post-synthesis treatments. This review highlights the progress in the understanding of fundamental mechanisms and issues associated with water splitting, influencing factors of MXenes, their value addition role, and application strategies for water splitting, including performance, challenges, and outlook of MXene-based photo-/electrocatalysts, in the last five years.

Preparation of sp2 carbon-bonded π-conjugated COF aerogels by ultrasound-assisted mild solvothermal reaction for multi-functional applications.

Molding COFs into aerogels from monomers can establish interpenetrating spatial network structures on the centimeter scale that increase the accessibility of dominant pore channels and the convenience of real application, which radically gets rid of the difficult reprocessing problems of insoluble and non-fusible powder COFs. However, the construction of bulk COF structures and achieving crystallinity are often incompatible, especially with sp2 carbon-based COFs, whose powder synthesis has been quite demanding. Herein, for the first time, we report an efficient method to prepare sp2 carbon-linked π-conjugated DFB-TMTA-COF (DT-COF) aerogels by an ultrasound-assisted mild solvothermal technique and freeze-drying. Particularly, unlike the typical synthesis methods of vacuum deoxygenation, high temperature and long reaction time, crystalline DT-COF aerogels can be obtained by reacting at 90 °C for 48 h without vacuum sealing. The fluffy, hierarchical porous flower-shaped microsphere clustering of DT-COF aerogels contributes to excellent mechanical properties and better host-guest interactions, which are favorable to utilize the benefits of the highly conjugated structure of channels. As a proof of concept, DT-COF aerogels have been used in absorption, batteries, and sensors, demonstrating enhanced functionality and effectiveness.

Modular Synthesis of Tripeptide Analogs with an Aminobitriazole Skeleton Using Diynyl Benziodoxolone as a Trivalent Platform.

A new synthesis method of tripeptide analogs with an aminobitriazole skeleton was proposed. The method involves assembling three amino acid-derived modules at the amino group site and onto a triisopropylsilyl diynyl benziodoxolone by copper-catalyzed electrophilic diynylation of amino acid-derived sulfonamides, chemoselective azide-alkyne cycloadditions with amino acid-derived azides, and deprotection. Various complex aminobitriazoles substituted with pyrene, nucleoside, and N-acetylglucosamine were also synthesized. The produced aminobitriazoles have three sp3 chiral centers and a C-N axial chirality.

Biogenic synthesis of nickel cobaltite nanoparticles via a green route for enhancing the photocatalytic and electrochemical performances

Green synthesis aligns with the global demand for eco-friendly and sustainable technologies, reducing the dependency on harmful chemicals and high-energy processes typically used in conventional synthesis techniques. This study highlights a novel green synthesis route for nickel cobaltite nanoparticles (NiCO2O4 NPs) utilizing Hyphaene thebaica extract as a natural reducing and stabilizing agent. The synthesized NiCO2O4 NPs, with sizes ranging from 20 to 30 nm, exhibited uniform diamond-like structures as confirmed by SEM and TEM imaging. XRD analysis verified the polycrystalline nature of these nanoparticles, while EDS measurements confirmed the elemental composition of Ni and Co. The presence of functional groups was subsequently verified through FT-IR analysis, and Raman spectroscopy further confirmed phase formation. Electrochemical evaluations revealed significant pseudocapacitive behavior, showing a specific capacitance of 519 F/g, demonstrating their potential for high-performance supercapacitors. To further assess the applicability of the synthesized NiCO2O4 NPs, their photocatalytic activity against methylene blue (MB) dye was investigated, resulting in a 99% degradation rate. This impressive photocatalytic efficiency highlights their potential application in environmental remediation. Overall, this work underscores the significant potential of green synthesis methods in producing high-performance nanomaterials while simultaneously reducing environmental impact and promoting sustainable development.

Covalent triazine frameworks (CTFs) drive innovative advances in rechargeable metal-ion batteries: a review

In the field of energy storage technology, the organic electrodes, separators, and electrolytes have unique advantages over inorganic materials, such as low cost, environmental friendliness, and a wide range of applications. Due to the advantages of organics such as light elements, abundant reserves, and recyclability, they have become favorable candidate materials for solving the energy storage problems caused by the fossil energy crisis. In recent years, as a high-performance branch of covalent organic frameworks, covalent triazine structures (CTFs) have attracted great interest due to their applications in electrochemical energy storage. CTFs have gradually become excellent organic materials for metal-ion batteries applications due to their large specific surface area, nitrogen richness, customizable structural features, and electron donor-acceptor/conductive parts. However, the relatively poor conductivity of the triazine ring in the main structure and the harsh polycondensation conditions limit its commercial application. To overcome these challenges, many effective strategies have emerged in terms of structural optimization, functional construction, and triazine-based composites. This review summarizes in detail the synthesis methods and applications of CTFs cathodes, electrolytes, and separators in the past decade. It is found that for CTFs, large-scale synthesis methods and performance regulation strategies have reached a bottleneck. It is hoped that the systematic summary of this review will provide strategic screening and prospects for the further expansion of CTFs research in next-generation batteries.

Ceramics with Ultrahigh Permittivity Values: Compositions, Synthesis Methods, and Properties at Low and Medium Frequencies

Ceramics with Ultrahigh Permittivity Values: Compositions, Synthesis Methods, and Properties at Low and Medium Frequencies

A comprehensive review on Nanoparticle: Characterization, classification, synthesis method, silver nanoparticles and its applications

Nanotechnology offers many advantages in various fields of science. Recent advances in nanotechnology have proven that nanoparticles acquire a great potential in medical applications. Recent advances in nanoscience and nanotechnology radically changed the way we diagnose, treat, and prevent various diseases in all aspects of human life. This present review provided a detailed overview of the synthesis, properties and applications of Nanoparticles (NPs) exist in different forms. NPs are tiny & small, ranges from 1 to 100 nm. They are classified into different classes based on their properties, shapes or sizes. The different groups include fullerenes, metal NPs, ceramic NPs, and polymeric NPs. NPs possess unique physical and chemical properties due to their high surface area and nanoscale size. Silver nanoparticles (AgNPs) are one of the most vital and fascinating nanomaterials among several metallic nanoparticles that are involved in biomedical applications. AgNPs play an important role in nanoscience and nanotechnology, particularly in nanomedicine. The major applications of silver nanoparticles in the medical field include diagnostic applications and therapeutic applications, apart from its antimicrobial activity.

Synthesis of New Complex Ferrite Li0.5MnFe1.5O4: Chemical–Physical and Electrophysical Research

In this article, the sol–gel method was used as a synthesis method, which shows the physicochemical nature of the synthesis of a new complex material, ferrite Li0.5MnFe1.5O4. The structure and composition of the synthesized ferrite were determined by X-ray phase analysis. According to analysis indicators, it was found that our compound is a single-phase, spinel-structured, and syngony-cubic type of compound. The microstructure of the compound and the quantitative composition of the elements contained within it were analyzed under a scanning electron microscope (SEM). Under a scanning electron microscope, microsystems were taken from different parts of Li0.5MnFe1.5O4-type crystallite; the elemental composition of crystals was analyzed; and the general type of surface layer of complex ferrite was shown. As a result, given the fact that the compound consists of a single phase, the clarity of its construction was determined by the topography and chemical composition of the compound. As a result, it was found that the newly synthesized complex ferrites correspond to the formula Li0.5MnFe1.5O4. The particles of the formed compounds have a large size (between 50.0 μm or 20.0 μm and 10.0 μm). Electrophysical measurements were carried out on an LCR-800 unit at intervals of 293–483 K and at frequencies of 1.5 and 10 kHz. An increase in frequency to 10 kHz led to a decrease in the value ε in the range of the studied temperature (293–483 K).

Accelerating evidence synthesis for safety assessment through ClinicalTrials.gov platform: a feasibility study

BackgroundStandard systematic review can be labor-intensive and time-consuming meaning that it can be difficult to provide timely evidence when there is an urgent public health emergency such as a pandemic. The ClinicalTrials.gov provides a promising way to accelerate evidence production.MethodsWe conducted a search on PubMed to gather systematic reviews containing a minimum of 5 studies focused on safety aspects derived from randomized controlled trials (RCTs) of pharmacological interventions, aiming to establish a real-world dataset. The registration information of each trial from eligible reviews was further collected and verified. The meta-analytic data were then re-analyzed by using 1) the full meta-analytic data with all trials and 2) emulated rapid data with trials that had been registered and posted results on ClinicalTrials.gov, under the same synthesis methods. The effect estimates of the full meta-analysis and rapid meta-analysis were then compared.ResultsThe real-world dataset comprises 558 meta-analyses. Among them, 56 (10.0%) meta-analyses included RCTs that were not registered in ClinicalTrials.gov. For the remaining 502 meta-analyses, the median percentage of RCTs registered within each meta-analysis is 70.1% (interquartile range: 33.3% to 88.9%). Under a 20% bias threshold, rapid meta-analyses conducted through ClinicalTrials.gov achieved accurate point estimates ranging from 77.4% (using the MH model) to 83.1% (using the GLMM model); 91.0% to 95.3% of these analyses accurately predicted the direction of effects.ConclusionsUtilizing the ClinicalTrials.gov platform for safety assessment with a minimum of 5 RCTs holds significant potential for accelerating evidence synthesis to support urgent decision-making.

Research Progress on the Preparation of Manganese Dioxide Nanomaterials and Their Electrochemical Applications

Manganese dioxide (MnO2) nanomaterials have shown excellent performance in catalytic degradation and other fields because of their low density and great specific surface area, as well as their tunable chemical characteristics. However, the methods used to synthesize MnO2 nanomaterials greatly affect their structures and properties. Therefore, the present work systematically illustrates common synthetic routes and their advantages and disadvantages, as well as examining research progress relating to electrochemical applications. In contrast to previous reviews, this review summarizes approaches for preparing MnO2 nanoparticles and describes their respective merits, demerits, and limitations. The aim is to help readers better select appropriate preparation methods for MnO2 nanomaterials and translate research results into practical applications. Finally, we also point out that despite the significant progress that has been made in the development of MnO2 nanomaterials for electrochemical applications, the related research remains in the early stages, and the focus of future research should be placed on the development of green synthesis methods, as well as the composition and modification of MnO2 nanoparticles with other materials.

Polyaniline-modified amorphous tin-based Prussian blue analogue as cathodes for long-life aqueous zinc ion batteries

Prussian blue analogs (PBAs) have emerged in the field of aqueous zinc ion batteries (AZIBs) owing to their simple synthesis method and three-dimensional open framework structure. Although PBAs have high redox potentials, the unsatisfactory specific capacity and poor electrical conductivity limit their development to some extent. In this work, amorphous tin hexacyanoferrate (SnHCF) and polyaniline (PANI) were combined to form SnHCF/PANI composite. The synergistic effect of the amorphous structure of SnHCF and PANI with good conductivity makes the SnHCF/PANI electrode exhibit excellent redox activity and achieve rapid ion/electron transfer. When used as a cathode in AZIBs, the SnHCF/PANI provides a high specific capacity (136.8 mAh g−1 at 0.5 A g−1) and excellent cycling stability (a discharge specific capacity of 54.3 mAh g−1 after 2500 cycles at 2 A g−1). This work offers a new idea for the development of PBAs-based composites as cathode materials for AZIBs.

Boosting energy storage via the strong interaction between Cu2O clusters and carbon rich framework

Metal oxides have attracted tremendous attention because of their easy fabrication, high reversible voltage, and decent electrochemical capacity in lithium ion batteries. However, the conversion of their structure and the low electric conductivity always lead to a high polarization and poor cyclic stability. Herein, the strong interaction between Cu2O and porous carbon-rich framework is constructed through an in-situ synthesis method. Benefit from the synergistic effect derived from this interaction, the confined size and the high reversibility in chemical reaction of Cu2O are realized. In the hybrid system, the conjugated carbon skeleton with acetylene bond plays crucial role not only in building strong interactions, but also in interconnecting numerous Cu2O clusters for the transport of charge and storing of ions in a homogeneous solid. Hence, the composite material of porous carbon-rich material and Cu2O electrode delivers a decent capacity of 804 and 305 mAh g–1 in lithium and sodium ion batteries, respectively. These results suggest the great potential of such carbon framework/metal oxides composite material applied for high performance battery.

Isovalent Co-Substitution of Iron and Titanium into Single-Crystal NMC622

Abstract Substitutional Li[Ni0.6Mn0.2Co0.2]O2 oxides (known as NMC622) were made by all-dry synthesis with Fe and Ti substituting Co and Mn, respectively. The substitutions were performed in three series, Fe substitution for Co, Ti substitution for Mn, and Fe and Ti co-substitution for Co and Mn, according to the formula Li(Ni0.6Mn0.2-yCo0.2-xFexTiy)O2. The resulting oxides were evaluated as cathode materials for Li-ion batteries. Fe-substitution for Co resulted in increased intersite mixing, resulting in increased polarization and capacity fade. Ti-substitution for Mn also resulted in increased intersite mixing, but the mixing was due to Ti3+ in the Li-layer. As a result, Ti-substituted NMCs had improved capacity retention and reduced polarization. These effects were independent of each other, so that Ti could partially offset the negative aspects of Fe-substitution. Additionally, layered Mn-free Li(Ni0.6Ti0.2Co0.2)O2 (NTC622) was produced as an endmember of this series for the first time with low intersite mixing and superior electrochemical performance in comparison to previous reports. These results demonstrate benefits of all-dry Ti-substitution in NMC and the all-dry synthesis method as an avenue towards new cathode composition discovery.

Paracetamol Inclusion in Mechanically Interlocked Nanocages.

The solid-state synthesis and fast crystallization under kinetic control of poly-[n]-catenanes self-assembled of mechanically interlocked metal organic cages (MOCs) is virtually unexplored. This is in part, due to the lack of suitable crystals for single crystal X-ray diffraction (SC-XRD) analysis which limits their progress as advanced functional materials. Here we report the unprecedented inclusion of paracetamol in the cavities of amorphous materials constituted of M12L8, interlocked MOCs synthesized by mechanochemistry under kinetic control. Full structure determination of a low-crystallinity and low-resolution powders of the M12L8 poly-[n]-catenane including paracetamol has been carried out combining XRD data and Density Functional Theory (DFT) calculations using a multi-step approach. Each M12L8 cage contains six paracetamol guests which is confirmed by thermal analysis and NMR spectroscopy. The paracetamol loading has been also carried out by the instant synthesis method using a saturated paracetamol solution in which TPB and ZnI2 self-assemble immediately (i. e., 1-5 seconds) encapsulating ~7 paracetamol molecules in the M12L8 nanocages under kinetic control also giving a good selectivity. Benzaldehyde has been included in the M12L8 cages using amorphous M12L8 polycatenanes showing that the icosahedral cages can serve as potential nanoreactors for instance to study Henry reactions in the solid-state.

A Combined Theoretical and Experimental Raman Scattering Study of BaZrS3-BaHfS3 Solid Solutions.

Ba(Zr,Hf)S3 solid solutions are proposed for photovoltaic applications and a fast non-destructive measurement of the composition of these solutions and the identification of any possible secondary phases is a prerequisite for understanding their opto-electronic properties. Here we calculate the non-resonant one-phonon Raman spectra of pure BaHfS3 and BaZrS3, which show only subtle differences between them. To test this experimentally, a solution series of BaZr1-xHfxS3 (0≤x≤1) powders was synthesised and free of a secondary phase, HfS3 identified by 633 nm excitation Raman spectroscopy. The veracity of the synthesis method was confirmed by comparing X-ray diffractograms and optical absorption spectra of the BaZr0.5Hf0.5S3 solid solution to a 50:50 mixture of the pure ternary compounds. Experimental non-resonant Raman measurements on the solid solution powders confirm that only slight variations in the spectra are visible, making a solid solution composition determination difficult. However, exciting the solid solutions resonantly, leads to the appearance of new two-phonon modes in the Raman spectrum, which change significantly across the solid solution series. We consequently suggest that a rapid solid solution composition measurement can be made unambiguously by measuring the ratio of the intensities of the 825 cm-1 and 625 cm-1 Raman features.

Direct Hydrothermal Synthesis and Characterization of Zr–Ce-Incorporated SBA-15 Catalysts for the Pyrolysis Reaction of Algal Biomass

In recent years, algae have emerged as a promising feedstock for biofuel production, due to their eco-friendly, sustainable, and renewable nature. Various methods, including chemical, biochemical, and thermochemical processes, are used to convert algal biomass into biofuels. Pyrolysis, a widely recognized thermochemical technique, involves high temperature and pressure to generate biochar and bio-oil from diverse algal sources. Various pyrolytic processes transform algal biomass into biochar and bio-oil, including low pyrolysis, fast pyrolysis, catalytic pyrolysis, microwave-assisted pyrolysis, and hydropyrolysis. These methods are utilized to convert a range of microalgae and cyanobacteria into biochar and bio-oil. In this publication, we will discuss catalytic pyrolysis using mesoporous materials, such as SBA-15. Mesoporous catalysts have earned significant attention for catalytic reactions, due to their high surface area, facilitating the better distribution of impregnated metal. Pyrolysis conducted in the presence of a mesoporous catalyst is viewed more as efficient, compared to reactions occurring within the smaller microporous cavities of traditional zeolites. SBA-15 supports with incorporated Zr and/or Ce were synthesized using the direct hydrothermal synthesis method. The catalyst was characterized using structural and morphological technical analysis and utilized for the pyrolysis reaction of the algal biomass.

Synthesis, characterization, and practical applications of perovskite quantum dots: recent update.

This review paper provides an in-depth analysis of Perovskite quantum dots (PQDs), a class of nanomaterials with unique optical and electronic properties that hold immense potential for various technological applications. The paper delves into the structural characteristics, synthesis methods, and characterization techniques of PQDs, highlighting their distinct advantages over other Quantum Dots (QDs). Various applications of PQDs in fields such as solar cells, LEDs, bioimaging, photocatalysis, and sensors are discussed, showcasing their versatility and promising capabilities. The ongoing advancements in PQD research and development point towards a bright future for these nanostructures in revolutionizing diverse industries and technologies.