Search Results (179)

An anion exchange-assisted technique was used for the synthesis of platinum-decorated SnO₂ supports, providing nanocatalysts with enhanced activity for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP). In this study, a series of SnO₂ supports, namely SnA (synthesized almost at room temperature), SnB (hydrothermally treated at 180 °C), and SnC (annealed at 600 °C), are systematically investigated, all loaded with 1 mol% Pt from H₂PtCl₆ under identical mild conditions. The chloride ions from the SnCl₄ precursors were efficiently removed via a strong-base anion exchange reaction, resulting in highly dispersed, crystalline ~5 nm cassiterite SnO₂ particles. All Pt/SnO₂ composites displayed mesoporous structures with type IVa isotherms and H₂-type hysteresis, with SP1a (Pt on SnA) exhibiting the largest surface area (122.6 m²/g) and the smallest pores (~3.5 nm). STEM-HAADF imaging revealed well-dispersed PtOx domains (~0.85 nm), while XPS confirmed the dominant Pt⁴⁺ and Pt²⁺ species, with ~25% Pt⁰ likely resulting from photoreduction and/or interactions with Sn–OH surface groups. Raman spectroscopy revealed three new bands (260–360 cm⁻¹) that were clearly visible in the sample with 10 mol% Pt and were due to the vibrational modes of the PtOx species and Pt-Cl bonds introduced due the addition and hydrolysis of H₂PtCl₆ precursor. TGA/DSC analysis revealed the highest mass loss for SP1a (~7.3%), confirming the strong hydration of the PtOx domains. Despite the predominance of oxidized PtOx species, SP1a exhibited the highest catalytic activity (k_app = 1.27 × 10⁻² s⁻¹) and retained 84.5% activity for the reduction of 4-NP to 4-AP after 10 cycles. This chloride-free low-temperature synthesis route offers a promising and generalizable strategy for the preparation of noble metal-based nanocatalysts on oxide supports with high catalytic activity and reusability. Full article

Vanadium dioxide (VO₂) is a phase-change material of great importance due to its thermochromic properties, which make it a potential candidate for energy-saving applications. In this work, a comparative study between VO₂ thermochromic films prepared from powders synthesized by either a lab-scale hydrothermal autoclave or a large-scale hydrothermal reactor is presented. In both cases, the as-obtained material, after the hydrothermal step, was subsequently annealed at 700 °C under a nitrogen atmosphere, in order to obtain the monoclinic VO₂(M) thermochromic phase. The VO₂ powder prepared in the large-scale hydrothermal reactor exhibited a critical transition temperature of 54 °C with a hysteresis width of 9 °C, while for the one prepared in the lab-scale autoclave, the respective values were 62 °C and 5 °C. Despite these differences, the prepared films showed similar thermochromic performance with the lab-scale material displaying a 17% IR (InfraRed), switching at 2000 nm upon heating, and a transmittance solar modulation of 11%, compared to 17% and 9%, respectively, for the large-scale material. Moreover, both films appeared to have similar luminous transmittance of 44% and 46%, respectively, at room temperature (25 °C). These results showcase the potential for scaling up the hydrothermal synthesis of VO₂, resulting in films with similar thermochromic performance to those from lab-scale fabrication. Full article

Tungsten-doped vanadium dioxide (W-VO₂) shows semiconductor-to-metal phase transition properties at room temperature, which is an ideal thermo-chromic smart window material. However, low visual transmittance and solar modulation limit its application in building energy saving. In this paper, a W-VO_2−x@AA core-shell nanoparticle is proposed to improve the thermo-chromic performance of W-VO₂. Oxygen vacancies were used to promote the connection of W-VO_2−x nanoparticles with L-ascorbic acid (AA) molecules. Oxygen vacancies were tuned in W-VO₂ nanoparticles by thermal annealing temperatures in vacuum, and W-VO_2−x@AA nanoparticles were synthesized by the hydrothermal method. A smart window was formed by dispersing W-VO_2−x@AA core-shell nanoparticles into PVP evenly and spin-coating them on the surface of glass. The visual transmittance of this smart window reaches up to 67%, and the solar modulation reaches up to 12.1%. This enhanced thermo-chromic performance is related to the electron density enhanced by the AA surface molecular coordination effect through W dopant and oxygen vacancies. This work provides a new strategy to enhance the thermo-chromic performance of W-VO₂ and its application in the building energy-saving field. Full article

In this study, we investigate the optical and structural properties of Cu-doped β-Ga₂O₃ nanostructures synthesized via a hydrothermal method, followed by annealing in ambient O₂. Different Cu doping concentrations (0, 1.6, and 4.8 at.%) are introduced to examine their effects on the crystal structure, chemical state, and optical bandgap of β-Ga₂O₃. X-ray diffraction (XRD) analysis reveals that the host β-Ga₂O₃ crystal structure is preserved at lower doping levels, whereas secondary phases (Ga₂CuO₄) appear at higher doping concentrations (4.8 at.%). X-ray photoelectron spectroscopy (XPS) confirms the presence of Cu²⁺ ions in both lattice substitution sites and surface-adsorbed hydroxylated species (Cu(OH)₂). The optical bandgap of β-Ga₂O₃ is found to decrease with increasing Cu concentration, likely due to the formation of localized states or secondary phases. These findings demonstrate the tunability of the optical properties of β-Ga₂O₃ via Cu doping, providing insights into the incorporation mechanisms and their impact on structural and electronic properties. Full article

This study employed a hydrothermal method to prepare V-doped MoS₂. The influence of varying filler ratios (30 wt%, 40 wt%, 50 wt%) on its absorption properties was analyzed. For annealing studies, a precursor powder with a 40 wt% filler ratio was heat-treated at 600 °C for 2 h. The results obtained through characterization and testing indicate that the unannealed 40 wt% filler sample demonstrates superior absorption performance, with minimum reflection loss (RL_min) of −32.24 dB, an effective absorption bandwidth (EAB) of 4.40 GHz, and 99.9% electromagnetic (EM) wave attenuation. However, upon subjecting the sample with a 40 wt% filling ratio to annealing treatment, a notable decrease in impedance matching degree was observed, and regions with impedance matching values close to 1 were no longer present. Consequently, it can be concluded that at a filling ratio of 40 wt%, the sample’s excellent attenuation coefficient in conjunction with its good impedance matching collectively contribute to its superior comprehensive absorption performance. Full article

In photoelectrochemical (PEC) biosensing, efficient electron-hole separation is crucial to obtain preferred photocurrent response and analytical performance; thus, constructing developed heterointerfaces with high carrier transfer efficiency is an effective method for sensitive evaluation of analytes. Herein, a 1D ZnIn₂S₄ nanosheet-decorated 2D In₂O₃ tube was developed to integrate with a prostate antigen (PSA)-sensitive aptamer for sensitive PSA antigen detection. 1D In₂O₃ tubes were first prepared by two-step hydrothermal and annealing methods, followed by the in-situ growth of ZnIn₂S₄ nanosheets. Morphology, optical properties, structure, and PEC performance of prepared In₂O₃-ZnIn₂S₄ were characterized by scanning electron microscopy, transmission electron microscopy, ultraviolet–visible spectrophotometry, X-ray diffraction, X-ray photoelectron spectroscopy, and an electrochemical workstation. Benefiting from the photoelectric effect and specific 1D/2D hierarchical structure, In₂O₃-ZnIn₂S₄ displayed enhanced optical absorption and photocarrier separation, thus a superior photoelectrochemical response. Proposed bioassay protocol possessed a linear range from 0.001 to 50 ng/mL and a detection limit at 0.00037 ng/mL. In addition, this biosensor exhibited satisfactory anti-interface ability and stability, which also could be extended to other quantitative platforms for detecting other proteins. Full article

Magnetic materials with intriguing structural and functional modifications demonstrate broad application potential in various fields, including drug delivery, absorption, extraction, separation, and catalysis. In particular, the catalytic hydrogenation of functionalized organic nitro compounds represents a significant research focus in contemporary catalysis studies. A facile synthesis of Fe₃O₄@C–Pt core-shell nanocatalysts was developed in this work through a sequential process involving (1) one-pot hydrothermal synthesis followed by N₂-annealing to obtain the Fe₃O₄@C core and (2) subsequent solvothermal deposition of platinum nanoparticles. Comprehensive characterization was performed using FT-IR, XRD, Raman spectroscopy, TEM, XPS, BET surface area analysis, TGA, and VSM techniques. The resulting magnetic nanocatalysts exhibited uniformly dispersed Pt nanoparticles and demonstrated exceptional catalytic performance in nitroarene hydrogenation reactions. Remarkably, the system showed excellent functional group tolerance across all 20 substituted nitroarenes, consistently yielding corresponding aromatic amine products with >93% conversion efficiency. Furthermore, the magnetic responsiveness of Fe₃O₄@C–Pt enabled convenient catalyst recovery through simple magnetic separation, with maintained catalytic activity over 10 consecutive reuse cycles without significant performance degradation. Full article

Hydrogen sensors play a crucial role in ensuring safety in various industrial applications. In this study, we demonstrated the use of a room-temperature hydrogen gas sensor based on Pt-nanoparticle-decorated TiO₂ nanorods (TiO₂ NRs/Pt NP). The TiO₂ NRs were synthesized via a hydrothermal method, followed by Pt deposition using sputtering and thermal annealing. Under UV illumination, the TiO₂ NR/Pt NP gas sensor exhibited a remarkable response of 2.4 at a 1% hydrogen concentration, which is approximately 5.9 times higher than that of bare TiO₂ NRs measured in the dark. This enhancement is attributed to the synergistic effect of Pt NPs, which promote charge separation and spillover for oxygen molecules, and UV activation, which generates additional carriers. Moreover, the sensor demonstrated stable and reliable detection of hydrogen concentrations up to 1% without the need for external heating, underscoring its practical applicability under ambient conditions. These results demonstrate that TiO₂ NRs/Pt NP, combined with UV activation, provide a promising approach for highly sensitive and room-temperature hydrogen detection, offering significant potential for hydrogen monitoring and hydrogen energy systems. Full article

Nanocrystalline materials based on titanium dioxide possess unique properties, including photocatalytic and antibacterial activities. Despite many approaches have already been utilized to fabricate and characterize pure and doped TiO₂, a systematic description of its nanostructured samples depending on the synthesis method has not been presented yet. In this study, we shed new light on the process–structure relationships of nanocrystalline TiO₂-based powders fabricated by extraction–pyrolytic, hydrothermal, and sol–gel techniques. The comprehensive analysis of the fabricated nanocrystalline TiO₂-based powders with different anatase/rutile phase content is performed by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). The hydrothermal and sol–gel methods are also used to grow TiO₂ particles doped with Cu and Er-Yb. The correlation between synthesis parameters (pyrolysis and annealing temperature) and properties of the produced materials is studied. Particular attention is paid to Raman spectroscopy and the detailed comparison of our obtained data with existing experimental and theoretical studies. Full article

A facile solvo-hydrothermal method was used to synthesize sub-100 nm diameter TiO₂/α-Fe₂O₃@SiO₂ nanorods (TiO₂/HNRs@SiO₂). Thermal annealing of TiO₂/HNRs@SiO₂ activated the photosensitizing crystalline TiO₂ domains containing mixed anatase and rutile phases. The photocatalytic degradation of methylene blue (MB), conducted using thermally annealed TiO₂/HNRs@SiO₂ photocatalysts, was successfully demonstrated with ~95% MB removal efficiency under mild conditions of pH = ~7 and room temperature using ~150 min of solar irradiation. The enhanced removal efficiency was attributed to the rapid adsorption of MB onto the TiO₂/HNRs@SiO₂ surface via favorable electrostatic interactions and the synergistic integration of α-Fe₂O₃ and TiO₂ into nanorod heterostructures with bandgaps of 1.99–2.03 eV, allowing them to absorb visible light for efficient photocatalytic decomposition. This study provides insights into designing photocatalysts with improved selectivity for sustainable water treatment and environmental remediation. Full article

Gallium oxide (Ga₂O₃), an ultrawide bandgap semiconductor, is an ideal material for solar-blind photodetectors, but challenges such as low responsivity and response speed persist. In this paper, one-dimensional (1D) Ga₂O₃ nanorods were designed to achieve high photodetection performance due to their effective light absorption and light field confinement. Through modulating source concentration, pH value, temperature, and reaction time, 1D β-Ga₂O₃ nanorods were controllably fabricated using a cost-effective hydrothermal method, followed by post-annealing. The nanorods had a diameter of ~500 nm, length from 0.5 to 3 μm, and structure from nanorods to spindles, indicating that different β-Ga₂O₃ nanorods can be utilized controllably through tuning reaction parameters. The 1D β-Ga₂O₃ nanorods with a high length-to-diameter ratio were chosen to construct metal-semiconductor-metal type photodetectors. These devices exhibited a high responsivity of 8.0 × 10⁻⁴ A/W and detectivity of 4.58 × 10⁹ Jones under 254 nm light irradiation. The findings highlighted the potential of 1D Ga₂O₃ nanostructures for high-performance solar-blind ultraviolet photodetectors, paving the way for future integrable deep ultraviolet optoelectronic devices. Full article

Electrochemical glucose sensors are vital for clinical diagnostics and the food industry, where accurate detection is essential. However, the limitations of glucose oxidase (GOx)-based sensors, such as complex preparation, high cost, and environmental sensitivity, highlight the need for non-enzymatic sensors that directly oxidize glucose at the electrode surface. In this study, a self-supporting hierarchical Cu/Fe₃O₄ nanosheet electrode was successfully fabricated by in situ growth on Ni Foam using a hydrothermal method, followed by annealing treatment. The Cu/Fe₃O₄ hierarchical nanosheet structure, with its large surface area, provides abundant active sites for electrocatalysis, while the strong interactions between Cu/Fe₃O₄ and Ni Foam enhance electron transfer efficiency. This novel electrode structure demonstrates exceptional electrochemical performance for non-enzymatic glucose sensing, with an ultrahigh sensitivity of 12.85 μA·μM⁻¹·cm⁻², a low detection limit of 0.71 μM, and a linear range extending up to 1 mM. Moreover, the Cu/Fe₃O₄/NF electrode exhibits excellent stability, a rapid response (~3 s), and good selectivity against interfering substances such as uric acid, ascorbic acid, H₂O₂, urea, and KCl. It also shows strong reliability in analyzing human serum samples. Therefore, Cu/Fe₃O₄/NF holds great promise as a non-enzymatic glucose sensor, and this work offers a valuable strategy for the design of advanced electrochemical electrodes. Full article

Non-noble metal electrocatalysts for the hydrogen oxidation reaction (HOR) that are both highly active and low-cost are essential for the widespread use of fuel cells. Herein, a simple two-step method for creating an in-plane heterostructure of Ni₃N/MoSe₂ loaded on N-doped reduced graphene oxide (Ni₃N/MoSe₂@N-rGO) as an effective electrocatalyst for the HOR is described. The process involves hydrothermal treatment of the Ni and Mo precursors with N-doped reduced graphene oxide, followed by the annealing with urea. The Ni₃N/MoSe₂@N-rGO catalyst exhibits high activities for the HOR, with current densities of 2.15 and 3.06 mA cm⁻² at 0.5 V vs. the reversible hydrogen electrode (RHE) in H₂-saturated 0.1 M KOH and 0.1 M HClO₄ electrolytes, respectively, which is comparable to a commercial 20% Pt/C catalyst under similar experimental conditions. Furthermore, the catalyst demonstrates excellent durability, maintaining its performance during accelerated degradation tests for 5000 cycles. This work offers a practical framework for the designing and preparing of non-precious metal electrocatalysts for the HOR in fuel cells. Full article

Thin films of gadolinium-doped ceria (GDC) nanoparticles were fabricated as electrolytes for low-temperature solid oxide fuel cells (SOFCs) by combining electrophoretic deposition (EPD) and the successive ionic layer adsorption and reaction-air spray plus (SILAR-A+) method. The Ce_1−xGd_xO_2−x/2 solid solution was synthesized using hydrothermal (HY) and solid-state (SS) procedures to produce high-quality GDC nanoparticles suitable for EPD fabrication. The crystalline structure, cell parameters, and phases of the GDC products were analyzed using X-ray diffraction. Variations in oxygen vacancy concentrations in the GDC samples were achieved through the two synthetic methods. The ionic conductivities of pressed pellets from the HY, SS, and commercial G_0.2DC samples, measured at 150 °C, were 0.6 × 10⁻⁶, 2.6 × 10⁻⁶, and 2.9 × 10⁻⁶ S/cm, respectively. These values were determined using electrochemical impedance spectroscopy (EIS) with a simplified equivalent circuit method. The morphologies of G_0.2DC thin films prepared via EPD and SILAR-A+ processes were characterized, with particular attention to surface cracking. Crack-free GDC thin films, approximately 730–1200 nm thick, were successfully fabricated on conductive substrates through the hybridization of EPD and SILAR-A+, followed by hydrothermal annealing. EIS and ionic conductivity (1.39 × 10⁻⁹ S/cm) measurements of the G_0.2DC thin films with thicknesses of 733 nm were performed at 300 °C. Full article

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 (I_D/I_G) in graphene sheets assisted in assessing the quality of the graphene films. An estimation of the number of structural defects was calculated using the I_D/I_G ratio. The Raman analysis showed an increase in the I_D/I_G 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