Search Results (122)

Transition metal (TM)-doped zinc oxide (ZnO) and zirconium dioxide (ZrO₂) nanocrystals exhibit complex correlations between crystal structure, defect chemistry, vibrational properties, and magnetic behavior that are strongly governed by synthesis route and dopant incorporation mechanisms. This review critically summarizes recent progress on Fe-, Mn-, and Co-doped ZnO and ZrO₂ nanocrystals synthesized by wet chemical, hydrothermal, and microwave-assisted hydrothermal methods, with emphasis on synthesis-driven phase evolution and apparent solubility limits. ZnO and ZrO₂ are treated as complementary host lattices: ZnO is a semiconducting, piezoelectric oxide with narrow solubility limits for most 3d dopants, while ZrO₂ is a dielectric, polymorphic oxide in which transition metal doping may stabilize tetragonal or cubic phases. Structural and microstructural studies using X-ray diffraction, electron microscopy, Raman spectroscopy, and Mössbauer spectroscopy demonstrate that at low dopant concentrations, TM ions may be partially incorporated into the host lattice, giving rise to diluted or defect-mediated magnetic behavior. When solubility limits are exceeded, nanoscopic secondary oxide phases emerge, leading to superparamagnetic, ferrimagnetic, or spin-glass-like responses. Magnetic measurements, including DC magnetization and AC susceptibility, reveal a continuous evolution from paramagnetism in lightly doped samples to dynamic magnetic states characteristic of nanoscale magnetic entities. Vibrational spectroscopy highlights phonon confinement, surface optical phonons, and disorder-activated modes that sensitively reflect nanocrystal size, lattice strain, and defect populations, and often correlate with magnetic dynamics. Rather than classifying these materials as diluted magnetic semiconductors, this review adopts a synthesis-driven and correlation-based framework that links dopant incorporation, local structural disorder, vibrational fingerprints, and magnetic response. By emphasizing multi-technique characterization strategies required to distinguish intrinsic from extrinsic magnetic contributions, this review provides practical guidelines for interpreting magnetism in TM-doped oxide nanocrystals and outlines implications for applications in photocatalysis, sensing, biomedicine, and electromagnetic interference (EMI) shielding. Full article

In this study, hydroxyapatite was synthesized using a microwave-assisted hydrothermal method. Calcium nitrate tetrahydrate (Ca(NO₃)₂·4H₂O) and ammonium phosphate ((NH₄)₂HPO₄) served as precursors in a pH 10 ammonium hydroxide (NH₄OH) solution. Polyvinylpyrrolidone (PVP) was employed as a surfactant at varying concentrations of 0 (M0), 0.1% (M1), 0.2% (M2), and 0.3%wt (M3) to control particle size and morphology. The synthesized samples were characterized using Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR). The addition of PVP during synthesis resulted in Ca/P ratios ranging from 0.93 to 1.37, and promoted predominantly rod-like morphologies. Samples M1 and M3 exhibited average diameters of 11.23–104.24 nm and lengths of 47.21–222.32 nm. XRD analysis confirmed the presence of both hexagonal and monoclinic phases, with crystallite sizes varying from 18.66 to 22.49 nm. FTIR spectra of sample M1 revealed an elongation at 3432 cm⁻¹ corresponding to OH⁻ groups, indicative of water absorption within the material structure. Vibrational bands at 2950–2300, 1090, and 975 cm⁻¹, attributed to C–H bonds in PVP were also identified. These findings highlight the influence of PVP concentration on the structural and morphological properties of hydroxyapatite, providing insights into its potential applications in various fields. Full article

Microwave heating has a good number of advantages in the synthesis of inorganic compounds when opportunely exploited. A deep knowledge of the interaction of the electromagnetic waves and matter is necessary to optimize irradiation of the reactor vessel so as to obtain homogeneous heating for homogeneous nucleation and growth of particles, localized heating of starting self-sustained high-temperature synthesis, and generation of a superfast heating and cooling profile to obtain metastable crystals. Case studies of pure oxides, mixed oxides, composites, phosphates, zeolites, and high-entropy alloys are discussed in the international frame of the academic and industrial research covering the last 20 years of microwave chemistry where Italian researchers covered a relevant role. Full article

Monitoring nitrogen dioxide (NO₂) in various scenarios is crucial due to its significant environmental impact as a hazardous gas which is emitted by several industrial sectors. This study reports the optimized synthesis of WO₃ flower-like structures using the microwave-assisted hydrothermal method under various experimental conditions, resulting in the optimized sample designated MF-WO₃-K2. Structural, morphological, and chemical characterizations revealed that WO₃ microflowers (MF-WO₃-K2) exhibit a hexagonal crystalline phase, a bandgap of 2.4 eV, and a high specific surface area of 61 m²/g. The gas-sensing performance of WO₃ microflowers was investigated by electrical measurements of six similarly fabricated MF-WO₃-K2 sensors. The MF-WO₃-K2 sensors demonstrated a remarkable sensor signal of 225 for 5 ppm NO₂ at 150 °C and response/recovery times of 14.5/2.4 min, coupled with outstanding selectivity against potential interfering gases such as CO, H₂, C₂H₂, and C₂H₄. Additionally, the sensors achieved a low detection limit of 65 ppb for NO₂ at 150 °C. The exceptional sensing properties of WO₃ microflowers are attributed to the abundance of active sites on the surface, large specific surface area, and the presence of pores in the material that facilitate the diffusion of NO₂ molecules into the structure. Overall, the WO₃ microflowers demonstrate a promising ability to be used as a sensitive layer in high-performance chemiresistive gas sensors due to their high sensor performance and good reproducibility for NO₂ detection. Full article

The manufacturing techniques, structural features, and optical attributes of titanium dioxide (TiO₂) nanoparticles are highlighted in this study. These nanoparticles are notable for their remarkable photocatalytic activity, cheap cost, chemical stability, and biocompatibility. TiO₂ consists of three polymorph structures: anatase, rutile, and brookite. Because of its electrical characteristics and large surface area, anatase is the most efficient for photocatalysis when exposed to UV light. The crystallinity, size, and shape of titania nanoparticles (NPs) are influenced by diverse production techniques. Sol-gel, hydrothermal, solvothermal, microwave-assisted, and green synthesis with plant extracts are examples of common methods. Different degrees of control over morphology and surface properties are possible with each approach, and these factors ultimately affect functioning. For example, microwave synthesis provides quick reaction rates, whereas sol-gel enables the creation of homogeneous nanoparticles. XRD and SEM structural investigations validate nanostructures with crystallite sizes between 15 and 70 nm. Particle size, synthesis technique, and annealing temperature all affect optical characteristics such as bandgap (3.0–3.3 eV), fluorescence emission, and UV-visible absorbance. Generally speaking, anatase has a smaller crystallite size and a greater bandgap than rutile. TiO₂ nanoparticles are used in gas sensing, food packaging, biomedical coatings, dye-sensitized solar cells (DSSCs), photocatalysis for wastewater treatment, and agriculture. Researchers are actively exploring methods like adding metals or non-metals, making new composite materials, and changing the surface to improve how well they absorb visible light. Full article

Carbon dots (CDs) have emerged as promising nanomaterials for optical sensing due to their outstanding photoluminescence, chemical stability, and biocompatibility. In recent years, the development of sustainable CDs derived from biomass—particularly cellulose—has attracted increasing interest as a green alternative to conventional synthetic routes. This review offers a comprehensive overview of recent advances in synthesis, functionalization, and application of cellulose-based carbon dots for environmental sensing. We examine key synthetic approaches—including hydrothermal, microwave-assisted, and pyrolytic methods—and discuss how the structure and origin of cellulose influence the physicochemical properties of the resulting CDs. The mechanisms underlying their sensing performance are analyzed in detail, with a focus on the detection of heavy metals, organic pollutants, and other environmental contaminants. Challenges related to reproducibility, scalability, and long-term stability are critically addressed. Finally, we outline future directions involving hybrid nanomaterials, real-time sensing platforms, and strategies aligned with circular economy principles. This review aims to serve as a valuable resource for researchers in the fields of sustainable nanomaterials, green chemistry, and environmental sensor development. Full article

This study investigates the structural and magnetic properties of CoFe₂O₄ nanoparticles prepared by five different synthesis methods: coprecipitation, ultrasound-assisted coprecipitation, coprecipitation coupled with mechanochemical treatment, microemulsion and microwave-assisted hydrothermal synthesis. The produced powders were additionally functionalized with starch to improve biocompatibility and colloidal stability. The starch-coating procedure itself by sonication in starch solution, as well as its result, affects the structural and magnetic properties of functionalized nanoparticles. The resulting changes of properties in the process of ligand addition depend significantly on the starting nanoparticles, or rather, on the method of their synthesis. The structural, magnetic and spectroscopic properties of the resulting materials were systematically investigated using X-ray diffraction (XRD), Raman spectroscopy, Mössbauer spectroscopy and magnetic measurements. Taken together, XRD, Raman and Mössbauer spectroscopy show that starch deposition reduces structural disorder and internal stress, resulting in nanoparticles with a more uniform size distribution. These changes, in turn, affect all magnetic properties—magnetization, coercivity and magnetic anisotropy. Magnetic responses are preserved what is desirable for future biomedical applications. This work emphasizes the importance of surface modification for tailoring the properties of magnetic nanoparticles while maintaining their desired functionality. Full article

Carbon microspheres were prepared by microwave-assisted hydrothermal treatment, at 180 °C, of commercial carbohydrates (saccharose, glucose, and xylose) and xylose extract obtained from almond shells with varying synthesis parameters. When 1.6 M aqueous solutions of commercial carbohydrates were used, 2–10 μm carbon microspheres were obtained from saccharose after 15 min, while a longer amount of time (60 min) and the addition of acid medium (1% v/v H₂SO₄, 1% v/v H₃PO₄) were needed to obtain carbon microspheres from commercial xylose and glucose (≤ 1 μm). The higher reactivity of saccharose could be related to the formation, during heating, of fructose, which is more reactive than glucose and xylose. An increase in the acid concentration and in the carbohydrate concentration increased the formation and size of the microspheres. Comparative experiments with conventional heating did not produce a solid. Interestingly, when xylose extract obtained from almond shells was used, small carbon microspheres (1–3 μm) were obtained at a much lower concentration (0.2 M) and time (15 min) than with commercial xylose. This could be related to the acid medium used during extraction of xylose from the biomass. Activation of microspheres with CO₂ resulted in high-surface area materials (243–326 m²/g) with great potential as catalytic supports. Full article

AuQDs (Au quantum dots) are ultrasmall nanostructures that combine the size-tunable fluorescence and photostability of semiconductor quantum dots with the chemical stability, low toxicity, and versatile surface chemistry of gold nanoparticles. This unique combination endows AuQDs with exceptional biocompatibility and multifunctionality, making them ideal for biomedical applications such as cellular imaging, real-time tracking, targeted drug delivery, diagnostics, therapeutic monitoring, and biosensing. Various synthesis methods—including chemical reduction, hydrothermal, laser ablation, and microwave-assisted techniques—allow for precise control over size and surface properties, optimizing fluorescence and electronic behavior for high-resolution imaging and sensitive detection. Compared to traditional quantum dots, AuQDs offer enhanced safety and biocompatibility, while surpassing larger gold nanoparticles by enabling fluorescence-based imaging. Their surfaces can be functionalized with diverse ligands for targeted delivery and specific biological interactions. In summary, AuQDs are multifunctional nanoprobes that combine superior optical properties, chemical stability, and biocompatibility, making them powerful tools for advanced biomedical diagnostics, therapy, and biosensing. Full article

One of the main challenges in hydroxyapatite research is to develop cost-effective synthesis methods that consistently produce materials closely resembling natural bone, while maintaining high biocompatibility, phase purity, and mechanical stability for biomedical applications. Traditional synthetic techniques frequently fail to provide desirable mechanical characteristics and antibacterial activity, necessitating the development of novel strategies based on natural precursors and selective ion doping. The present study aims to explore the possibility of synthesizing hydroxyapatite through the co-precipitation method, followed by a microwave-assisted hydrothermal maturation process. The main CaO sources selected for this study are eggshells and mussel shells. Cu²⁺ and Sr²⁺ ions were added into the hydroxyapatite structure at concentrations of 1% and 5% to investigate their potential for biomedical applications. Furthermore, the morpho-structural and biological properties have been investigated. Results demonstrated the success of hydroxyapatite synthesis and ion incorporation into its chemical structure. Moreover, HAp samples exhibited significant antimicrobial properties, especially the samples doped with 5% Cu and Sr. Additionally, all samples presented good biological activity on MC3T3-E1 osteoblast cells, demonstrating good cellular viability of all samples. Therefore, by correlating the results, it could be concluded that the undoped and doped hydroxyapatite samples are suitable biomaterials to be further applied in orthopedic applications. Full article

This study reports the synthesis and evaluation of iron molybdate (Fe₂(MoO₄)₃) and iron tungstate (FeWO₄) as photocatalysts for the degradation of a real industrial effluent from aluminum anodizing processes under visible light irradiation. The oxides were synthesized via a co-precipitation method in an aqueous medium, followed by microwave-assisted hydrothermal treatment. Structural and morphological characterizations were performed using X-ray diffraction, field-emission scanning electron microscopy, Raman spectroscopy, ultraviolet–visible (UV–vis), and photoluminescence (PL) spectroscopies. The effluent was characterized by means of ionic chromatography, total organic carbon (TOC) analysis, physicochemical parameters (pH and conductivity), and UV–vis spectroscopy. Both materials exhibited well-crystallized structures with distinct morphologies: Fe₂(MoO₄)₃ presented well-defined exposed (001) and (110) surfaces, while FeWO₄ showed a highly porous, fluffy texture with irregularly shaped particles. In addition to morphology, both materials exhibited narrow bandgaps—2.11 eV for Fe₂(MoO₄)₃ and 2.03 eV for FeWO₄. PL analysis revealed deep defects in Fe₂(MoO₄)₃ and shallow defects in FeWO₄, which can influence the generation and lifetime of reactive oxygen species. These combined structural, electronic, and morphological features significantly affected their photocatalytic performance. TOC measurements revealed degradation efficiencies of 32.2% for Fe₂(MoO₄)₃ and 45.3% for FeWO₄ after 120 min of irradiation. The results highlight the critical role of morphology, optical properties, and defect structures in governing photocatalytic activity and reinforce the potential of these simple iron-based oxides for real wastewater treatment applications. Full article

Aquatic biomass—ranging from fish scales and crustacean shells to various algae species—offers an abundant, renewable source for carbon dot (CD) synthesis, aligning with circular economy principles. This review highlights recent studies for valorizing aquatic biomass into high-performance carbon-based nanomaterials—specifically aquatic biomass-based carbon dots (AB-CDs)—briefly summarizing green synthesis approaches (e.g., hydrothermal carbonization, pyrolysis, and microwave-assisted treatments) that minimize environmental impact. Subsequent sections highlight the varied applications of AB-CDs, particularly in biosensing (including the detection of marine biotoxins), environmental monitoring of water pollutants, and drug delivery systems. Physically AB-CDs show unique optical and physicochemical properties—tunable fluorescence, high quantum yields, enhanced sensitivity, selectivity, and surface bio-functionalization—that make them ideal for a wide array of applications. Overall, the discussion underlines the significance of this approach; indeed, transforming aquatic biomass into carbon dots can contribute to sustainable nanotechnology, offering eco-friendly solutions in sensing, environmental monitoring, and therapeutics. Finally, current challenges and future research directions are discussed to give a perspective of the potential of AB-CDs; the final aim is their integration into multifunctional, real-time monitoring and therapeutic systems—for sustainable nanotechnology innovations. Full article

Magnetic zeolite nanocomposites (NCs) have emerged as a promising class of hybrid materials that combine the high surface area, porosity, and ion exchange capacity of zeolites with the magnetic properties of nanoparticles (NPs), particularly iron oxide-based nanomaterials. This review provides a comprehensive overview of the synthesis, characterization, and diverse applications of magnetic zeolite NCs. We begin by introducing the fundamental properties of zeolites and magnetic nanoparticles (MNPs), highlighting their synergistic integration into multifunctional composites. The structural features of various zeolite frameworks and their influence on composite performance are discussed, along with different interaction modes between MNPs and zeolite matrices. The evolution of research on magnetic zeolite NCs is traced chronologically from its early stages in the 1990s to current advancements. Synthesis methods such as co-precipitation, sol–gel, hydrothermal, microwave-assisted, and sonochemical approaches are systematically compared, emphasizing their advantages and limitations. Key characterization techniques—including X-Ray Powder Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning and Transmission Electron Microscopy (SEM, TEM), Thermogravimetric Analysis (TGA), Nitrogen Adsorption/Desorption (BET analysis), Vibrating Sample Magnetometry (VSM), Zeta potential analysis, Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES), and X-Ray Photoelectron Spectroscopy (XPS)—are described, with attention to the specific insights they provide into the physicochemical, magnetic, and structural properties of the NCs. Finally, the review explores current and potential applications of these materials in environmental and biomedical fields, focusing on adsorption, catalysis, magnetic resonance imaging (MRI), drug delivery, ion exchange, and polymer modification. This article aims to provide a foundation for future research directions and inspire innovative applications of magnetic zeolite NCs. Full article

Tomato waste (TW) was employed as a sustainable source for the synthesis of fluorescent carbon dots (CDs) via a microwave-assisted hydrothermal carbonization (Mw-HTC) method, aiming at its valorization. Several amines were used as nitrogen additives to enhance the fluorescence quantum yield (QY) of CDs, and a set of reaction conditions, including additive/TW mass ratio (0.04–0.32), dwell time (15–60 min), and temperature (200–230 °C) of the HTC process, were scrutinized. The structural analysis of the tomato waste carbon dots (TWCDs) was undertaken by FTIR and ¹H NMR techniques, revealing their most relevant features. In solid state, transmission electron microscopy (TEM) analysis showed the presence of nearly spherical nanoparticles with an average lateral size of 8.1 nm. Likewise, the topographical assessment by atomic force microscopy (AFM) also indicated particles’ heights between 3 and 10 nm. Their photophysical properties, revealed by UV–Vis, steady-state, and time-resolved fluorescence spectroscopies, are fully discussed. Higher photoluminescent quantum yields (up to 0.08) were attained when the biomass residues were mixed with organic aliphatic amines during the Mw-HTC process. Emission tunability is a characteristic feature of these CDs, which display an intensity average fluorescence lifetime of 8 ns. The new TWCDs demonstrated good antioxidant properties by the ABTS radical cation method (75% inhibition at TWCDs’ concentration of 5 mg/mL), which proved to be related to the dwell time used in the CDs synthesis. Moreover, the synthesized TWCDs suppressed the growth of Escherichia coli and Staphylococcus aureus at concentrations higher than 2000 μg/mL, encouraging future antibacterial applications. Full article

The electrical conductivity of nanocrystalline CuMnO₂ samples, obtained by microwave-assisted hydrothermal synthesis (MWH), is studied by impedance spectroscopy over a frequency range of 30 Hz to 2 MHz and a temperature range from 30 to 120 °C. Three samples are prepared to start from a mixture of sulphate reactants, at two synthesis temperatures and different reaction times (of applying microwaves): sample S1 at 80 °C for 5 min; sample S2 at 120 °C for 5 min and sample S3 at 120 °C for one hour. The static conductivity values, σ_DC of samples S2 and S3, are approximately equal but larger than those of sample S1. This result suggests that using MWH synthesis at 120 °C, with different reaction times (samples S2 and S3), is sufficient for microwaves to be applied for at least 5 min to obtain samples with similar electrical properties. The experimental data were analysed based on three theoretical models, demonstrating that the most appropriate theoretical model to explain the electrical conduction mechanism in the samples is Mott’s variable range hopping (VRH) model. Using this model, the activation energy of conduction, (E_A,cond), the density of localized states near the Fermi level, N(E_F), the hopping distance, R_h(T), the hopping energy, W_h(T) and the charge carrier mobility (μ) were determined for the first time, for microwave-assisted hydrothermally synthesized crednerite. Additionally, the band gap energy (W_m) and hopping frequency (ω_h) were evaluated at various temperatures T. Understanding the electrical conduction mechanism in the polycrystalline CuMnO₂ materials is important for their use in photo-electrochemical and photocatalytic applications, photovoltaic devices, and, more recently, in environmental protection. Full article