Search Results (82)

A facile and versatile strategy to obtain NPs@ZnAlO nanocomposite materials, comprising controlled-size nanoparticles (NPs) within a ZnAlO matrix is reported. The mono-(Au, Ni) and bimetallic (Ni-Au) NPs serving as an active phase were prepared by the polyol-alkaline method, while the ZnAlO support was obtained via the thermal decomposition of its corresponding layered double hydroxide (LDH) precursors. X-ray diffraction (XRD) patterns confirmed the successful fabrication of the nanocomposites, including the synthesis of the metallic NPs, the formation of LDH-like structure, and the subsequent transformation to ZnO phase upon LDH calcination. The obtained nanostructures confirmed the nanoplate-like morphology inherited from the original LDH precursors, which tended to aggregate after the addition of gold NPs. According to the UV-Vis spectroscopy, loading NPs onto the ZnAlO support enhanced the light absorption and reduced the band gap energy. ATR-DRIFT spectroscopy, H₂-TPR measurements, and XPS analysis provided information about the functional groups, surface composition, and reducibility of the materials. The catalytic performance of the developed nanostructures was evaluated by the photodegradation of bisphenol A (BPA), under simulated solar irradiation. The conversion of BPA over the bimetallic Ni-Au@ZnAlO reached up to 95% after 180 min of irradiation, exceeding the monometallic Ni@ZnAlO and Au@ZnAlO catalysts. Its enhanced activity was correlated with good dispersion of the bimetals, narrower band gap, and efficient charge carrier separation of the photo-induced e⁻/h⁺ pairs. Full article

Transition metal oxides (TMOs) are considered to be highly promising materials for supercapacitor electrodes due to their low cost, multiple convertible valence states, and excellent electrochemical properties. However, inherent limitations, including restricted specific surface area and low electrical conductivity, have largely restricted their application in supercapacitors. In this paper, core–shell heterostructures of nickel–iron layered double hydroxide (NiFe-LDH) nanosheets uniformly grown on CuCo₂O₄ nanoneedles were synthesized by hydrothermal and calcination methods. It is found that the novel core–shell structure of CuCo₂O₄@NiFe-LDH improves the electrical conductivity of the electrode materials and optimizes the charge transport path. Under the synergistic effect of the two components and the core–shell heterostructure, the CuCo₂O₄@NiFe-LDH electrode achieves an ultra-high specific capacity of 323.4 mAh g⁻¹ at 1 A g⁻¹. And the capacity retention after 10,000 cycles at 10 A g⁻¹ is 90.66%. In addition, the assembled CuCo₂O₄@NiFe-LDH//RGO asymmetric supercapacitor device achieved a considerable energy density (68.7 Wh kg⁻¹ at 856.3 W kg⁻¹). It also has 89.36% capacity retention after 10,000 cycles at 10 A g⁻¹. These properties indicate the great potential application of CuCo₂O₄@NiFe-LDH in the field of high-performance supercapacitors. Full article

Mixed oxides were obtained via calcination at 550 °C from layered double hydroxides (LDHs), which were synthesized in a previous study via co-precipitation and co-precipitation followed by hydrothermal treatment using aluminum residues as the source of this element. After characterization, these oxides (Mg-Al-_LDH-CP and Mg-Al-_LDH-H, named according to the synthesis methods of the precursor LDHs) were applied as heterogeneous catalysts in the methyl transesterification of ethyl acetate (EA). The formation of mixed oxides was confirmed by the absence of basal peaks associated with the layered LDH structure in the XRD analysis, due to calcination. Further characterization revealed that Mg-Al-_LDH-CP exhibited the highest number of acidic sites, while Mg-Al-_LDH-H had the highest number of basic sites. The transesterification activity was evaluated in the reaction between ethyl acetate (EA) and methanol (MeOH). The best result, obtained under a molar ratio of 1:5:0.005 (EA:MeOH:catalyst) at 120 °C, was a 63% conversion after 360 min of reaction for the Mg-Al-_LDH-CP catalyst, which had a higher number of acidic sites and fewer basic sites. Additionally, the catalysts demonstrated robustness, maintaining catalytic activity over four cycles without a significant decrease in performance. These results indicate the feasibility of using mixed oxides derived from LDH, synthesized from aluminum residues, as heterogeneous catalysts in transesterification reactions, highlighting their potential for advancing more sustainable catalyst development. Full article

The pyrolysis carbon black (CBp) from waste tires contains zinc, iron, and other metal elements, which have high recycling value. This study proposes a simple method of recovering zinc and iron from waste tire-derived CBp to synthesize hydrotalcite-type adsorbents for the treatment of anodic dye wastewater. Firstly, zinc-aluminum hydrotalcite (LDH) and zinc-iron aluminum hydrotalcite (FeLDH) were obtained by leaching the zinc and iron ions from CBp with an acid solution. As compared with LDH, FeLDH shows increased laminate metal ion arrangement density and layer spacing. By calcining the LDH and FeLDH at 500 °C, zinc aluminum oxides (LDO) and zinc iron aluminum oxides (FeLDO) were then prepared and applied for the adsorption of dye methyl orange (MO). The results demonstrate that the maximum adsorption capacity of LDO and FeLDO are 304.9 and 609.8 mg g⁻¹ at pH of 4.0, respectively. The adsorption processes of both LDO and FeLDO are consistent with the Langmuir adsorption isotherm and the proposed second-order kinetic model. The adsorption regeneration performance and adsorption mechanism of LDO and FeLDO were also investigated in detail. Regeneration experiments show that after three cycles, the removal rate of MO by LDO remains above 80%, while that of FeLDO only remains around 64% in the first cycle after regeneration. This work would provide a new pathway to realize the high-value metal recycling of waste tire-derived CBp and solve the contamination of dye wastewater. Full article

This study aimed to synthesize a multicationic hydrotalcite and transform it into mixed oxide nanostructures (ZnO/TiO₂/CeO₂/Al₂O₃, referred to as MixO) to serve as a heterogeneous photocatalyst for degrading various pollutants, including methylene blue (MB), methyl orange (MO), paracetamol (PA), and paraquat (PQ). The hydrotalcite was synthesized via an ultrasound-assisted method and calcined at 700 °C to obtain the corresponding mixed metal oxide. A comprehensive characterization of both the multicationic hydrotalcite (MC-LDH) and the mixed metal oxides (MixO) was performed using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), N₂ adsorption–desorption, Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and pH_PZC analysis. The MixO sample exhibited an optical bandgap of 3.19 eV. Photocatalytic performance was evaluated during 240 min of UV irradiation, demonstrating high degradation efficiencies attributable to the synergistic interactions among ZnO, TiO₂, and CeO₂. Degradation efficiencies reached 99.3% for MO and 95.2% for MB, while PA and PQ showed moderate degradation rates of 60% and 15%, respectively. The degradation kinetics of all pollutant compounds followed the Langmuir–Hinshelwood model. Additionally, the MixO catalyst maintained consistent performance over four consecutive degradation cycles, highlighting its reusability and stability. These findings underscore the potential of MixO mixed oxide nanostructures as practical and recyclable photocatalysts for environmental remediation, particularly in wastewater treatment applications. Full article

In this study, zinc–aluminum layered double hydroxide (ZLDH) and its calcined counterpart (CZLDH) were synthesized and incorporated into a poly(vinylidene fluoride) (PVDF) matrix to develop high-performance anti-corrosion coatings for mild steel substrates. The structural integrity, morphology, and dispersion of the LDH fillers were analyzed using FTIR, XRD, Raman spectroscopy, and SEM/EDS, while coating performance was evaluated through water contact angle (WCA), adhesion tests, and electrochemical techniques. Comparative electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization tests in a 3.5% NaCl solution revealed that the ZLDH/PVDF coating exhibited superior corrosion resistance and long-term stability compared to CZLDH/PVDF and pristine PVDF coatings. The intact lamellar structure of ZLDH promoted excellent dispersion within the polymer matrix, enhancing interfacial adhesion, reducing porosity, and effectively blocking chloride ion penetration. Conversely, calcination disrupted the lamellar structure of ZLDH, reducing its compatibility and adhesion performance within the PVDF matrix. This study demonstrates the critical role of ZLDH’s structural integrity in achieving enhanced adhesion, barrier properties, and corrosion protection, offering an effective anti-corrosion coating for marine applications. Full article

A layered double hydroxide (LDH) containing Mg and Al was synthesized from a nitrate solution using a coprecipitation method. The resulting material exhibited a homogeneous structure, which, upon calcination at 450 °C, was converted into a layered double oxide (LDO). When rehydrated in a fluoride-containing aqueous solution, the original hydroxide structure was successfully regenerated, demonstrating the LDH’s memory effect. During this transformation, fluoride anions from the solution were incorporated into the interlayer galleries to maintain electroneutrality, as confirmed by energy-dispersive X-ray spectroscopy (EDS) analysis. Separately, the process was tested in the presence of ethanol, which significantly enhanced the incorporation of fluoride ions into the interlayer spaces. The material’s potential for controlled fluoride release was evaluated by monitoring its release into demineralized water. For comparison, a simple ion-exchange process was carried out using the as-synthesized MgAl LDH. The memory effect mechanism displayed a notably higher fluoride incorporation capacity compared to the ion-exchange process. Among all the specimens, the sample reconstructed in the presence of ethanol exhibited the highest fluoride ion content. Fluoride release studies revealed a two-phase pattern: an initial rapid release within the first three hours, followed by a substantially slower release over time. Full article

Engineering magnetic nanoparticles with tunable structural properties and magnetism is critical to develop desirable magnetic particle imaging (MPI) tracers for biomedical applications. Here we present a new superparamagnetic metal oxide nanoparticle with a controllable chemical composition and magnetism for imaging tumor xenografts in living mice. Superparamagnetic Zn/Fe mixed metal oxide (ZnFe-MMO) nanoparticles are fabricated via a facile one-pot co-precipitation method in water followed by thermal decomposition with tunable Zn/Fe ratios and at various calcination temperatures. This work, for the first time, presented LDH-derived metal oxides for an MPI application. The metal composition is tunable to present an optimized MPI performance. The analytical results demonstrate that ZnFe-MMO nanoparticles at the designed molar ratio of Zn/Fe = 2:1 after 650 °C calcination demonstrate a higher saturation magnetization (M_S) value and optimal MPI signal than the samples presented with other conditions. The excellent biocompatibility of ZnFe-MMO is demonstrated in both breast cancer cells and fibroblast cell cultures. In vivo imaging of 4T1 tumor xenografts in mice using ZnFe-MMO as a tracer showed that the mean signal intensity is 1.27-fold higher than the commercial tracer VivoTrax at 72 h post-injection, indicating ZnFe-MMO’s promise for prolonged MPI imaging applications. Full article

Phenolic antioxidants such as tert-butylhydroquinone (TBHQ) can prolong the shelf life of edible oils by delaying the oxidation process. The excessive use of TBHQ can damage food quality and public health, so it is necessary to develop an efficient TBHQ detection technique. In this work, nickel-aluminum double hydroxide (NiAl-LDH) was grown on glucose carbon spheres (GC), which formed porous carbon nanomaterials (named NiAl-LDH@GC-800) after pyrolysis at 800 °C. The successful synthesis of the material was verified by scanning electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. The obtained NiAl-LDH@GC-800 was dopped onto a glass carbon electrode to prepare an electrochemical sensor for TBHQ. The synergistic effect of porous carbon and Ni metal reduced from NiAl-LDH by high-temperature calcination accelerated the electron transfer rate and improved the sensitivity of the sensor. The prepared sensor showed a low limit of detection (LOD) of 8.2 nM, a high sensitivity (4.2 A·M⁻¹), and a good linear range (20~300 µM) in detecting TBHQ. The sensor was also successfully used for TBHQ detection in edible oils, including chili oil, peanut oil, and rapeseed oil. Full article

Layered double hydroxides (LDHs) and their derived mixed oxides are emerging as a promising class of biocompatible inorganic lamellar nanomaterials. The detailed structure and textural characteristics of the synthesized LDH-based materials were examined using X-ray diffraction, Fourier transform infrared spectroscopy, and N₂ adsorption/desorption isotherm. This study explored the removal efficiency of pharmaceutical tolperisone hydrochloride (TLP), as well as the herbicides quinmerac (QUI) and clomazone (CLO) from water, using dried and calcined LDH-based photocatalysts under simulated solar irradiation and UV irradiation. A higher removal efficiency was observed using UV irradiation, for all substrates. The most effective removal was achieved using ZnAl photocatalysts thermally treated at 100 °C (ZnAl 100) and 500 °C (ZnAl 500). The highest removal rates were observed in the TLP/ZnAl 100 and QUI/ZnAl 100 systems, achieving ~79% and ~86% removal after 75 min of treatment under UV. In contrast, the CLO/ZnAl 100 and CLO/ZnAl 500 systems achieved ~47% removal of CLO. Furthermore, this study investigated the role of reactive species to elucidate the mechanisms of photodegradation under UV. It was found that in the degradation of TLP and QUI in the presence of ZnAl 100 and ZnAl 500, the superoxide anion radical played the most important role. Full article

This research paper provides a comprehensive overview of the use of layered double hydroxides (LDH) in the removal of selenium species from contaminated water sources. Key studies on sorption mechanisms and the impact of competing ions on selenium removal are presented, and the effectiveness of LDH is compared across different structures and compositions. Scholarly sources extensively document the application of conventional LDH for effective selenium removal, with notable advancements achieved through innovative synthesis approaches. Comparative studies between LDH synthesized through various methods reveal the potential of tailored LDH for enhanced selenium adsorption. The paper further explores the influence of competing anions on LDH efficacy, emphasizing the impact of sulfate on selenium removal. Additionally, investigations into calcined LDH and commercially available variants underscore the potential for industrial applications. Beyond conventional LDH, the paper delves into iron-based LDH, LDH with intercalated thiomolybdate anions, and layered rare earth hydroxides, exploring their effectiveness in separating different selenium species. The role of pH in the removal of selenium species and the impact of three-metal cation LDH are also discussed. The study extends to nanocomposites, combining LDH with zero-valent iron, carbon-based materials, and organic compounds, illustrating their potential for selenium species immobilization. The presented findings offer valuable insights for researchers and practitioners in environmental science, addressing the growing demand for efficient selenium remediation strategies. Full article

In this investigation, Zn/Al carbonate layered double hydroxide (ZAC-LDH) and its derived material on calcination were synthesized for removing the anionic azo dye Congo red (CR) from wastewater. Numerous factors were methodically investigated, including temperature, adsorbent dosage, pH, starting Dye Concentration (DC), and contact time. The CR elimination percentage dropped as the initial DC increased from 25 mg/L to 100 mg/L at 30 °C for uncalcined LDH, and from 97.96% to 89.25% for calcined LDH. The pH analysis indicates that the highest level of dye removal was recorded within the acidic pH range through the electrostatic attraction mechanism. The sorption kinetics analysis results demonstrated that the pseudo-second-order kinetic model exhibited a stronger fit to both uncalcined LDH and CZA-LDH, with the maximum correlation coefficient value. The Van’t Hoff plots indicate the spontaneous nature of the physisorption process with a negative ΔG° (<−20 kJ/mol), while the endothermic adsorption process exhibited a positive ΔH°. The X-ray diffraction of calcined LDH reveals a significant intercalation of CR dye molecules, both prior to and following adsorption, showcasing a distinctive memory effect. The Brunauer–Emmett–Teller (BET) gas sorption measurements were performed to support the mesoporous nature of ZAC-LDH and CZA-LDH. The FTIR spectrum confirms the interaction of dye molecules on the surface of uncalcined and calcined LDH. These findings emphasize the efficacy of both the synthesized LDHs in removing CR dye, with CZA-LDH demonstrating superior efficiency compared to uncalcined LDH in the context of CR removal from wastewater. Full article

We developed a novel electrochemical sensor for the detection of alfuzosin (AFZ), a drug used to treat benign prostatic hyperplasia, using a double-shelled Co₃O₄/NiCo₂O₄ nanocomposite-modified electrode. The nanocomposites were synthesized using a template-assisted approach, with zeolitic imidazole framework-67 (ZIF-67) as the sacrificial template, involving the formation of uniform ZIF-67/Ni-Co layered double hydroxide (LDH) hollow structures followed by calcination to achieve the final nanocomposite. The nanocomposite was characterized by various techniques and showed high porosity, large surface area, and good conductivity. The nanocomposite-modified electrode exhibited excellent electrocatalytic activity towards AFZ oxidation, with a wide linear range of 5–180 µM and a low limit of detection of 1.37 µM. The sensor also demonstrated good repeatability, reproducibility, and stability selectivity in the presence of common interfering substances. The sensor was successfully applied to determine the AFZ in pharmaceutical tablets and human serum samples, with satisfactory recoveries. Our results suggest that the double-shelled Co₃O₄/NiCo₂O₄ nanocomposite is a promising material for the fabrication of electrochemical sensors for AFZ detection. Full article

The highly crystalline ZnAl layered double hydroxides (ZnAl-NO₃-LDHs) are utilized for the potential transformation into mixed metal oxides (MMOs) through thermal decomposition and used further for the photodegradation of phenol to assess the influence of calcination on ZnAl-LDHs with enhanced photoactivity. The structure, composition, and morphological evolution of ZnAl-LDHs to ZnO-based MMO nanocomposites, which are composed of ZnO and ZnAl₂O₄, after calcination at different temperatures (400–600 °C), are all thoroughly examined in this work. The final ZnO and ZnAl₂O₄-based nanocomposites showed enhanced photocatalytic activity. The findings demonstrated that calcining ZnAl-LDHs from 400 to 600 °C increased the specific surface area and also enhanced the interlayer spacing of d₀₀₃ while the transformation of LDHs into ZnO/ZnAl₂O₄ nanocomposites through calcining the ZnAl-LDH precursor at 600 °C showed significant photocatalytic properties, leading to complete mineralization of phenol under UV irradiation. Full article

Highly porous layered double hydroxide (LDH) and its calcined mixed metal oxide (MMO) were obtained by utilizing egg white (EW) as a biogenic porous template. The LDH was prepared through coprecipitation under the existence of a beaten EW meringue, and the corresponding MMO was obtained by calcining LDH at 500 °C. According to X-ray diffraction, the crystal structure of LDH and MMO was well-developed with or without EW. In contrast, the crystallinity analyses and microscopic investigations clearly showed differences in the particle orientation in the presence of EW; the protein arrangement in the EW foam induced the ordered orientation of LDH platelets along proteins, resulting in well-developed inter-particle pores. As a result, the distinctive particle arrangement in EW-templated samples compared with non-templated ones showed dramatically enhanced specific surface area and porosity. The nitrogen adsorption–desorption isotherm exhibited that the high specific surface area was attributed to the homogeneous nanopores in EW-templated LDH and MMO, which originated from the sacrificial role of the EW. Full article