Search Results (34)

Highly sensitive real-time detection of hydrogen sulfide (H₂S) is important for human health and environmental protection due to its highly toxic properties. The development of high-performance H₂S sensors remains challenging for poor selectivity, high limit detection and slow recovery from irreversible sulfidation. To solve these problems, we strategically prepared a layered structure of CuO-sensitized WO₃ flower-like hollow spheres with CuO as the sensitizing component. A 15 wt% CuO/WO₃ exhibits an ultra-high response (R_a/R_g = 571) to 10 ppm H₂S (131-times of pure WO₃), excellent selectivity (97-times higher than 100 ppm interference gas), and a low detection limit (100 ppb). Notably, its fast response (4 s) is accompanied by full recovery within 236 s. After 30 days of continuous testing, the response of 15 wt% CuO/WO₃ decreased slightly but maintained the initial response of 90.5%. The improved performance is attributed to (1) the p-n heterojunction formed between CuO and WO₃ optimizes the energy band structure and enriches the chemisorption sites for H₂S; (2) the reaction of H₂S with CuO generates highly conductive CuS, which significantly reduces the interfacial resistance; and (3) the hierarchical flowery hollow microsphere structure, heterojunction, and oxygen vacancy synergistically promote the desorption. This work provides a high-performance H₂S gas sensor that balances response, selectivity, and response/recovery kinetics. Full article

K–Se batteries offer high energy density and cost-effectiveness, making them promising candidates for energy storage systems. However, their practical applications are hindered by Se aggregation, sluggish ion diffusion, and significant volumetric expansion. To address these challenges, monodisperse hierarchical N-doped carbon microspheres (NCHS) with uniformly sized pores were synthesized as cathode hosts. The flower-like microstructure, formed by the assembly of two-dimensional building blocks, mitigated Se aggregation and facilitated uniform distribution within the pores, enhancing Se utilization. Nitrogen doping, introduced during synthesis, strengthened chemical bonding between selenium and the carbon host, suppressed side reactions, and accelerated reaction kinetics. These synergistic effects enabled efficient ion transport, improved electrolyte accessibility, and enhanced redox reactions. Additionally, the uniform particle and pore sizes of NCHS effectively mitigated volumetric expansion and surface accumulation, ensuring long-term cycling stability and superior electrochemical performance. Se-loaded NCHS (Se@NCHS) exhibited a high discharge capacity of 199.4 mA h g⁻¹ at 0.5 C after 500 cycles with 70.4% capacity retention and achieved 188 mA h g⁻¹ at 3.0 C, outperforming conventional carbon hosts such as Super P. This study highlights the significance of structural and chemical modifications in optimizing cathode materials and offers valuable insights for developing high-performance energy storage systems. Full article

CeO₂ has a potential application in the purification of organic dye wastewater because of the abundant oxygen vacancy (V_O) defects in its crystals. In this study, a cubic CeO₂ microsphere with layered interleaved symmetrical 3D flower-like morphology was synthesized, and its adsorption capacity for acid orange 7 (AO7) was further enhanced by Y doping. The impact of varying amounts of Y ions on the phase composition, lattice parameters, and morphology of the product was investigated, revealing that 4 mol.% was determined as the doping level limit of Y ions in CeO₂ crystals. XPS, Raman, and H₂−TPR techniques were employed to compare surface species changes before and after 4 mol.% Y doping in the CeO₂ crystals, including O−Ce(III), O−Ce(IV), O−Y(III), and V_O correlation, yielding a rough quantitative assessment of these species. The 4 mol.% Y-doped CeO₂ (2.0 g/L) demonstrated the highest removal rate for 20 mg/L of AO7 dye within just 20 min to reach adsorption–desorption equilibrium, half the time required by undoped CeO₂, achieving an impressive adsorption rate of 94.6%, compared to only 69.5% for undoped CeO₂ at 20 min. The adsorption capacity of undoped CeO₂ was enhanced by 19.05% through the doping of 4 mol.% Y, achieving a value of 16.56 mg/L. The feasibility of enhancing the adsorption capacity of CeO₂ by Y doping provides a reference for the application of CeO₂ and other metal oxides. Full article

This research introduces a non-enzymatic electrochemical sensor utilizing flower-like nickel oxide/carbon (fl-NiO/C) microspheres for the precise detection of L-glutamic acid (LGA), a crucial neurotransmitter in the field of healthcare and a frequently utilized food additive and flavor enhancer. The fl-NiO/C were synthesized with controllable microstructures using metal–organic frameworks (MOFs) as precursors followed by a simple calcination process. The uniformly synthesized fl-NiO/C microspheres were further characterized using Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX), and field emission scanning electron microscopy (FE-SEM). The fl-NiO/C was utilized as a modifier on the surface of a glassy carbon electrode, and an impedimetric sensor based on electrochemical impedance spectroscopy (EIS) was developed for the detection of LGA. The proposed sensor demonstrated excellent catalytic activity and selectivity towards LGA across a broad concentration range of 10–800 μM with a sensitivity of 486.9 µA.mM⁻¹.cm⁻² and a detection limit of 1.28 µM (S/N = 3). The sensor was also employed to identify LGA in blood plasma samples, yielding results that align with those obtained through HPLC. This achievement highlights the potential of fl-NiO/C microspheres in advancing cutting-edge biosensing applications. Full article

The synthesis of the accurate composition and morphological/structural design of multielement semiconductor materials is considered an effective strategy for obtaining high-performance hybrid photocatalysts. Herein, sulfur vacancy (Vs)-bearing In₂S₃/CuInS₂ microflower heterojunctions (denoted Vs-In₂S₃/CuInS₂) were formed in situ using In₂S₃ microsphere template-directed synthesis and a metal ion exchange-mediated growth strategy. Photocatalysts with flower-like microspheres can be obtained using hydrothermally synthesized In₂S₃ microspheres as a template, followed by Ostwald ripening growth during the metal cation exchange of Cu⁺ and In³⁺. The optimal heterostructured Vs-In₂S₃/CuInS₂ microflowers exhibited CO and CH₄ evolution rates of 80.3 and 11.8 μmol g⁻¹ h⁻¹, respectively, under visible-light irradiation; these values are approximately 4 and 6.8 times higher than those reported for pristine In₂S₃, respectively. The enhanced photocatalytic performance of the Vs-In₂S₃/CuInS₂ catalysts could be attributed to the synergistic effects of the following factors: (i) the constructed heterojunctions accelerate charge-carrier separation; (ii) the flower-like microspheres exhibit highly uniform morphologies and compositions, which enhance electron transport and light harvesting; and (iii) the vs. may trap excited electrons and, thus, inhibit charge-carrier recombination. This study not only confirms the feasibility of the design of heterostructures on demand, but also presents a simple and efficient strategy to engineer metal sulfide photocatalysts with enhanced photocatalytic performance. Full article

Thermocatalytic decomposition is an efficient purification technology that is potentially applicable to degrading chemical warfare agents and industrial toxic gases. In particular, ZrO₂ has attracted attention as a catalyst for the thermocatalytic decomposition of dimethyl methylphosphonate (DMMP), which is a simulant of the nerve gas sarin. However, the influence of the crystal phase and morphology on the catalytic performance of ZrO₂ requires further exploration. In this study, monoclinic- and tetragonal-phase ZrO₂ (m- and t-ZrO₂, respectively) with nanoparticle, flower-like shape and hollow microsphere morphologies were prepared via hydrothermal and solvothermal methods, and their thermocatalytic decomposition of DMMP was systematically investigated. For a given morphology, m-ZrO₂ performed better than t-ZrO₂. For a given crystalline phase, the morphology of hollow microspheres resulted in the longest protection time. The exhaust gases generated by the thermocatalytic decomposition of DMMP mainly comprised H₂, CO₂, H₂O and CH₃OH, and the by-products were phosphorus oxide species. Thus, the deactivation of ZrO₂ was attributed to the deposition of these phosphorous oxide species on the catalyst surface. These results are expected to help guide the development of catalysts for the safe disposal of chemical warfare agents. Full article

Flower-like cobalt–molybdenum mixed-oxide microspheres (CoMo-FMs) with hierarchical architecture were successfully synthesized via a hydrothermal process and subsequent calcination step. The characterization results show that CoMo-FMs were assembled from ultrathin mesoporous nanosheets with thicknesses of around 4.0 nm, providing the composite with a large pore volume and a massive surface area. The synthesized CoMo-FMs were employed as catalysts for the aerobic oxidative desulfurization (AODS) of fuel, and the reaction results show that the optimal catalyst (CoMo-FM-2) demonstrated an outstanding catalytic performance. Over CoMo-FM-2, various thiophenic sulfides could be effective removed at 80–110 °C under an atmospheric pressure, and a complete conversion of sulfides could be achieved in at least six consecutive cycles without a detectable change in chemical compositions. Further, the catalytic mechanism was explored by conducting systemic radical trapping and transformation experiments, and the excellent catalytic performance for CoMo-FMs should be mainly due to the synergistic effect of Mo and Co elements. Full article

Around a quarter of annual worldwide silver consumption comes from recycling. It remains a primary target for researchers to increase the silver ion adsorption capacity of the chelate resin. Herein, a series of flower-like thiourea–formaldehyde microspheres (FTFM) possessing diameters of 15–20 μm were prepared via a one-step reaction under acidic conditions, and the effects of the monomer molar ratio and reaction time on the micro-flower morphology, specific surface area, and silver ion adsorption performance were explored. The nanoflower-like microstructure showed the maximum specific surface area 18.98 ± 0.949 m²/g, which was 55.8 times higher than that of the solid microsphere control. As a result, the maximum silver ion adsorption capacity was 7.95 ± 0.396 mmol/g, which was 10.9 times higher than that of the control. Kinetic studies showed that the equilibrium adsorption amount of FT₁F₄M was 12.61 ± 0.016 mmol/g, which was 11.6 times higher than that of the control. Additionally, the isotherm study of the adsorption process was performed, and the maximum adsorption capacity of FT₁F₄M was 18.17 ± 1.28 mmol/g, which was 13.8 times that of the control according to the Langmuir adsorption model. Its high absorption efficiency, convenient preparation strategy, and low cost recommend FTFM bright for further use in industrial applications. Full article

Hierarchical organic structures have gained vast attention in the past decade owing to their great potential in chemical and medical applications in industries such as the food and pharmaceutical industries. In this paper, the crystallization of L-glu hierarchical spheres using inorganic ions, namely calcium, barium and strontium cations, is described. The anti-solvent precipitation method is used for the spherical crystallization. The L-glu microspheres are characterized using various techniques, including X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photo-electron microscopy (XPS) and polarized microscopy (POM). It is shown that without additives, L-glu crystallizes as flower-like structures, very different from the hierarchical spheres crystallized with the charged additives. Based on our results, we suggest a mechanism for the hierarchical sphere formation based on the crystallization and self-assembly of L-glu in emulsion droplets using charged additives. Full article

This study fabricated tantalum (Ta)-doped titanium dioxide with a unique nanorod-assembled actinomorphic-flower-like microsphere structured film. The Ta-doped TiO₂ actinomorphic-flower-like microsphere (TAFM) was fabricated via the solution immersion method in a Schott bottle with a home-made improvised clamp. The samples were characterised using FESEM, HRTEM, XRD, Raman, XPS, and Hall effect measurements for their structural and electrical properties. Compared to the undoped sample, the rutile-phased TAFM sample had finer nanorods with an average 42 nm diameter assembled to form microsphere-like structures. It also had higher oxygen vacancy sites, electron concentration, and mobility. In addition, a reversed double-beam photoacoustic spectroscopy measurement was performed for TAFM, revealing that the sample had a high electron trap density of up to 2.5 μmolg⁻¹. The TAFM showed promising results when employed as the resistive-type sensing film for a humidity sensor, with the highest sensor response of 53,909% obtained at 3 at.% Ta doping. Adding rGO to 3 at.% TAFM further improved the sensor response to 232,152%. Full article

Ultra-fine hydrogen produced by electrochemical water splitting without carbon emission is a high-density energy carrier, which could gradually substitute the usage of traditional fossil fuels. The development of high-performance electrocatalysts at affordable costs is one of the major research priorities in order to achieve the large-scale implementation of a green hydrogen supply chain. In this work, the development of a vanadium-doped FeBP (V-FeBP) microsphere croissant (MSC) electrocatalyst is demonstrated to exhibit efficient bi-functional water splitting for the first time. The FeBP MSC electrode is synthesized by a hydrothermal approach along with the systematic control of growth parameters such as precursor concentration, reaction duration, reaction temperature and post-annealing, etc. Then, the heteroatom doping of vanadium is performed on the best FeBP MSC by a simple soaking approach. The best optimized V-FeBP MSC demonstrates the low HER and OER overpotentials of 52 and 180 mV at 50 mA/cm² in 1 M KOH in a three-electrode system. In addition, the two-electrode system, i.e., V-FeBP || V-FeBP, demonstrates a comparable water-splitting performance to the benchmark electrodes of Pt/C || RuO₂ in 1 M KOH. Similarly, exceptional performance is also observed in natural sea water. The 3D MSC flower-like structure provides a very high surface area that favors rapid mass/electron-transport pathways, which improves the electrocatalytic activity. Further, the V-FeBP electrode is examined in different pH solutions and in terms of its stability under industrial operational conditions at 60 °C in 6 M KOH, and it shows excellent stability. Full article

In this work, flower-like molybdenum disulfide (MoS₂) microspheres were produced with polyethylene glycol (PEG) to form MoS₂-PEG. Likewise, gold nanoparticles (AuNPs) were added to form MoS₂-PEG/Au to investigate its potential application as a theranostic nanomaterial. These nanomaterials were fully characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), photoelectron X-ray spectroscopy (XPS), Fourier-transformed infrared spectroscopy (FTIR), cyclic voltammetry and impedance spectroscopy. The produced hierarchical MoS₂-PEG/Au microstructures showed an average diameter of 400 nm containing distributed gold nanoparticles, with great cellular viability on tumoral and non-tumoral cells. This aspect makes them with multifunctional characteristics with potential application for cancer diagnosis and therapy. Through the complete morphological and physicochemical characterization, it was possible to observe that both MoS₂-PEG and MoS₂-PEG/Au showed good chemical stability and demonstrated noninterference in the pattern of the cell nucleus, as well. Thus, our results suggest the possible application of these hybrid nanomaterials can be immensely explored for theranostic proposals in biomedicine. Full article

The development of non-noble Co₃O₄ catalysts exposing highly active crystal planes to low-temperature methane oxidation is still a challenge. Hence, a facile solvothermal method was adapted to construe flower-like Co₃O₄ hierarchical microspheres (Co₃O₄-FL), which are composed of nanosheets with dominantly exposed {112} crystal planes. The flower-like hierarchical structure not only promotes the desorption of high levels of active surface oxygen and enhances reducibility, but also facilitates an increase in lattice oxygen as the active species. As a result, Co₃O₄-FL catalysts offer improved methane oxidation, with a half methane conversion temperature (T₅₀) of 380 °C (21,000 mL g⁻¹ h⁻¹), which is much lower than that of commercial Co₃O₄ catalysts (Co₃O₄-C). This study will provide guidance for non-noble metal catalyst design and preparation for methane oxidation and other oxidative reactions. Full article

Porous structure and surface defects are important to improve the performance of supercapacitors. In this study, a facile pathway was developed for high-performance supercapacitors, which can produce transition metal hydroxides (LDHs) with abundant porous structure and surface defects. The NiCo-SDBS-LDH was prepared by one-step hydrothermal reaction using sodium dodecylbenzene sulfonate (SDBS) as anionic surfactant. And then, three dimensional (3D) interconnected porous flower-like 3D-NiCo-SDBS-LDH microspheres were designed and synthesized using the gas-phase hydrazine hydrate reduction method. Results showed that the hydrazine hydrate reduction not only introduces a large number of pores into 3D-NiCo-SDBS-LDH microspheres and causes the formation of oxygen vacancies, but it also roughens the surface of the microspheres. All these changes contribute to the enhancement of electrochemical activity of 3D-NiCo-SDBS-LDH; the NiCo-SDBS-LDH electrode after hydrazine hydrate treatment (3D-NiCo-SDBS-LDH) exhibits a higher specific capacitance of 1148 F·g⁻¹ at 1 A·g⁻¹ (about 1.46 times larger than that of NiCo-SDBS-LDH) and excellent long cycle life with 94% retention after 4000 cycles. Moreover, the assembled 3D-NiCo-SDBS-LDH//AC (active carbon) asymmetric supercapacitor (ASC) achieves remarkable energy density of 73.14 W h·kg⁻¹ at 800 W·kg⁻¹ and long-term cycling stability of 95.5% retention for up to 10,000 cycles. The outstanding electrochemical performance can be attributed to the synergy between the rich porous structure and the roughened surface that has been created by the hydrazine hydrate treatment. Full article

The practical application of photocatalytic H₂-evolution is greatly limited by its sluggish charge separation, insufficient active sites, and stability of photocatalysts. Zero-dimensional (0D) Ti₃C₂ MXene quantum dots (MQDs) and amorphous Ti(IV) have been proven to be potential substitutes for noble co-catalyst to accelerate the separation of photogenerated electron-hole pairs and prevent the self-oxidation of photocatalysts, leading to better photocatalytic H₂-evolution performance with long-term stability. In this study, amorphous Ti(IV) and MQDs co-catalysts were successfully deposited on ZnIn₂S₄ (ZIS) microspheres composed of ultra-thin nanosheets via a simple impregnation and self-assembly method (denoted as MQDs/ZIS/Ti(IV)). As expected, the optimal MQDs/ZIS/Ti(IV) sample exhibited a photocatalytic H₂-evolution rate of 7.52 mmol·g⁻¹·h⁻¹ and excellent photostability without metallic Pt as the co-catalyst in the presence of Na₂S/Na₂SO₃ as hole scavenger, about 16, 4.02 and 4.25 times higher than those of ZIS, ZIS/Ti(IV), and MQDs/ZIS, respectively. The significantly enhanced photocatalytic H₂-evolution activity is attributed to the synergistic effect of the three-dimensional (3D) flower-like microsphere structure, the amorphous Ti(IV) hole co-catalyst, and a Schottky junction formed at the ZIS–MQDs interface, which offers more active sites, suppresses self-photocorrosion, and photo-generates the charge recombination of ZIS. Full article