This paper reports a successful preparation of a pure forsterite Mg2SiO4 using the sol–gel approach and its application for the removal of impurities from a Tunisian frying oil. Magnesium nitrate hexahydrate and tetraethylortho-silicate were used as magnesium and silicon precursors, respectively. The synthesis was held at different calcination temperatures for 30?min. The annealed samples were characterized by X-ray diffraction, Fourier transform infrared, scanning electron microscopy, and laser diffraction. The results revealed that the sample calcined at 500?°C was forsterite with unimodal particle size distribution (PSD) centered at 122.8?±?0.3?μm. The dispersion index I (indicator of particle size uniformity) was 1.84. With the temperature increase, well crystallized compounds were obtained. Their PSDs remain unimodal and shift towards smaller particles. A decrease of the dispersion index was also noted, indicating the formation of Mg2SiO4 with more uniform particle size. This study showed that 900?°C could be selected as energy saving temperature suitable for the preparation of a pure and well crystallized Mg2SiO4 within just 30?min of annealing time. The obtained silicate exhibited promoting results for the purification of waste frying oils.
Pure and fine Mg2SiO4 powder with unimodal particle size distribution was prepared by sol gel route under energy saving conditions. The obtained magnesium orthosilicate showed excellent results for waste frying oil purification
The aim of this work was an investigation of structural and electrical properties of ZnO/Zn2-xFexTiO4 (x?=?0.7, 1, 1.4) powders. The compounds obtained by sol-gel method are characterized by several techniques: X-ray diffraction (XRD), N2 adsorption–desorption isotherms, scanning and transmission electron microscopy (SEM and TEM), X-ray photoelectron spectroscopy (XPS), electrical and dielectrical measurements. The XRD, SEM and XPS analysis confirmed the formation of ZnFeTiO4 inverse spinel structure. The electrical and dielectrical properties of ZnO/Zn2-xFexTiO4 (x?=?0.7, 1, 1.4) were measured by impedance spectroscopy, revealing a decrease in the electrical conductivity and the dielectric constant with Fe content.
Herein, porous Li3V2(PO4)3/C microspheres made of nanoparticles are obtained by a combination of sol spray-drying and subsequent-sintering process. Beta-cyclodextrin serves as a special chelating agent and carbon source to obtain carbon-coated Li3V2(PO4)3 grains with the size of ca. 30–50?nm. The unique porous structure and continuous carbon skeleton facilitate the fast transport of lithium ion and electron. The Li3V2(PO4)3/C microspheres offer an outstanding electrochemical performance, which present a discharge capacity of 122?mAh?g?1 at 2?C with capacity retention of 96% at the end of 1000 cycles and a high-rate capacity of 113?mAh?g?1 at 20?C in the voltage window of 3.0–4.3?V. Moreover, the Li3V2(PO4)3/C microspheres also give considerable cycling stability and high-rate reversible capacity at a higher end-of-charge voltage of 4.8?V.
MgF2 coating solutions were solvothermally treated at 160?°C for different time periods, this procedure induced crystallization and particle growth. Antireflection coatings prepared on glass from these solutions were compared to films derived from untreated precursor material. Ellipsometric porosimetry (EP) was employed to characterize structural features of coatings on glass as function of annealing temperature. Based on precursor solutions that had undergone solvothermal treatment antireflective coatings with a peak transparency exceeding 99% were prepared on PMMA substrates.
Solvothermal treatment of MgF2 precursor solutions results in crystallization of particles that can directly be applied to PMMA substrates for λ/4 antireflective films.
Bismuth ferrite (BiFeO3) nanopowder have been successfully synthesized for the first time via a microwave-assisted sol-gel combustion method by using citric acid as fuel. The resulting nanopowder was characterized using FT-IR, TG-DTA, XRD, EDX, VSM, SEM, and UV-Vis DRS. A ferromagnetic hysteresis loop with a saturation magnetization (MS) of 0.66?emu?g?1 has been observed at room temperature in the sample. The optical properties of the nanosized BiFeO3 showed its small band gap (=2.08?eV) indicates a possibility of utilizing much visible light for photocatalysis.
Phase pure, mesoporous, and crystalline V2O5 is synthesized by acid hydrolysis technique and subsequently heat treatment is carried out at 450, 500, 550, and 600?°C in air. The as-synthesized and heat-treated powders are thoroughly studied by X-ray diffraction, electron microscopy, dynamic light scattering, and spectroscopic techniques. A unique morphological tuning of V2O5 powders from as small as ~80?nm tiny nanorod to as large as a ~2.5?μm hexagonal grain as microstructural unit blocks is observed. A qualitative mechanism is suggested for particle growth. Further, the powders are pelletized and subsequently sintered in air at the same temperatures of 450, 500, 550, and 600?°C at which the powders were heat treated. Finally, nanomechanical properties of bulk pelletized V2O5 such as nanohardness and Young’s modulus are also evaluated by nanoindentation technique at nine different loads e.g., 10, 30, 50, 70, 100, 300, 500, 700, and 1000?mN.
Novel La-doped Bi2WO6 composites were successfully prepared via a facile solvothermal method and well characterized by X-ray diffraction, Brunner?Emmet?Teller measurements, scanning electron microscopy, transmission electron microscopy/high-resolution, energy dispersive spectrometry, X-ray photoelectron spectroscopy, ultraviolet–visible spectroscopy, and Fourier transform infrared spectroscopy. The photocatalytic activity of modified catalysts was evaluated by degrading tetracycline hydrochloride under visible light (450?W Xe lamp irradiation). It was found 5%La-Bi2WO6 had the highest light-absorption ability, great morphology, and microstructures. The La dopant enlarged surface area and increased crystal defects, which may enhance the optical absorption activity and inhibit the recombination of the photo-generated charge carrier, respectively. After 150?min illumination, the photocatalysts that 5%La-Bi2WO6 and pure Bi2WO6 exhibited the best and worst photocatalytic performance, respectively (96.25% vs. 88.92%).
In this study, the effective TiO2/Ag composite antibacterial aerogel powder is prepared by facile sol–gel method and ethanol supercritical technology. The surface morphology, structural properties, and chemical components are monitored by scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR), and energy disperse?spectroscopy (EDS). Meanwhile, absorbance spectra and specific surface area of TiO2/Ag composite aerogel are characterized by UV-Vis spectra and Brunauer–Emmett–Teller. The TiO2/Ag composite aerogel with Ti/Ag molar ratios of 10:1, 30:1, 50:1 are measured for its antibacterial property by using Escherichia coliform (E.coli) and Staphylococcus aureus (S. aureus). The results show that the size of TiO2 and Ag nanoparticles are 40?nm and 25?nm, respectively. Simultaneously, the obtained composite aerogel with a porous structure possessed a surface area of 148?m2/g, an average pore size 11.5?nm, and a pore volume 0.39?cm3/g. With the increase of Ag content, the antibacterial properties of composite aerogel are greatly improved compared with pure TiO2 aerogel. When Ag/Ti molar ratios was 1:10, the highest antibacterial rate can up to 99%, and the inhibition bands of E. coli and S. aureus are 23?mm and 19?mm, respectively.
Flower-like ceria (CeO2) architectures consisting of well aligned nanosheets were first synthesized by a glycol solvothermal method. The size of CeO2 architectures is about 5?μm in width and 10?μm in length, with the nanosheets thickness below 100?nm. Subsequently, the adsorbed Ag ions on the surface of CeO2 were in situ reduced to form Ag nanoparticles (NPs), leading to the fabrication of Ag/CeO2 hybrid architectures (HAs). The formed Ag NPs with sizes of 20–40?nm were uniformly loaded on the surface of the CeO2 sheets. The antibacterial properties of Ag/CeO2 HAs against Gram-negative E. coli and Gram-positive S. aureus were evaluated by minimum inhibitory concentration (MIC), minimum bactericidal concentration (MBC), and a filter paper inhibition zone method. The results demonstrated that Ag/CeO2 HAs displayed excellent antibacterial activity toward S. aureus and E. coli, which were attributed to the synergistic antibacterial effect between Ag NPs and CeO2 in HAs. Here, CeO2 nanoflowers as a new substrate could restrict Ag NPs aggregations and improve their antibacterial activities. Therefore, the resulted Ag/CeO2 HAs would be considered as a promising antibacterial agent.
CaMn7O12 precursor sol was prepared by using Ca(NO3)2·4H2O and Mn(CH3COO)4·4H2O as the raw materials, acetylacetone (AcAcH) as the chelating agent, and methyl alcohol (MeOH) as the solvent. The CaMn7O12 crystalline film was obtained via dip-coating and annealing treatment on the LaAlO3 (001) single-crystal substrate. XRD θ-2θ scan indicated that the as-prepared CaMn7O12 film had strong preferred orientation along the c-axis. In addition, the results of the ω and ? scans demonstrated that the film exhibited outstanding out-of-plane and in-plane texture characteristics. The SEM characterization showed that the CaMn7O12 film was dense and free of cracks. The grain size was uniform with an average size of ~180?nm. Vibrating sample magnetometer (VSM) test results indicated the CaMn7O12 film was antiferromagnetic and had a saturation magnetization of 114.2?emu/cm3 at 50?K.
Dual-network aerogels (HPSA) with improved mechanical property and thermal insulation were prepared by vacuum impregnation of HNTs/PVA aerogels (the first network aerogel, HPA) in tetraethoxysilane (TEOS). Scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy, and N2 adsorption–desorption analysis were used to study micromorphology and microstructure of HPSA, while compression tests and thermal conductivity tests were used to investigate related properties. The results showed that the dual-network frame was successfully constructed, this enabled HPSA to display enhanced compressive properties with increased HNTs content. The addition of silica sol improved the mesoporous characteristics including specific surface area and pore volume and also reduced the thermal conductivities. The first network made it possible for HPSA to possess good mechanical property, while SiO2 aerogel allowed HPSA greater thermal insulation. The obtained aerogel samples exhibited a high compressive strength (i.e., 1.36?MPa) and a low thermal conductivity (i.e., 0.022?W/(m?K)). HNTs/SiO2 dual-network aerogels with improved strength and thermal insulation could show great potential in a wide variety of applications.
As p–n heterojunction photocatalysts usually possess dramatically improved photocatalytic activity than single photocatalysts, a novel ZnO/Cu2O heterojunction was designed by a facile self-templating method in this study. The crystal structure, chemical composition, surface morphology, and optical property of ZnO/Cu2O heterojunction were investigated to clarify the structure-property correlation. Scanning electron microscope and transmission electron microscope images proved the uniform core-shell submicrospheres of ZnO/Cu2O, in which a three-dimensional flower-like ZnO core was coated by a shell comprised of Cu2O nanoparticles. The photoresponse result showed that the band gap of the ZnO/Cu2O core-shell submicrospheres became narrow, and the absorption edge shifted from the ultraviolet region (380?nm) to the visible region (500?nm) compared with the pure ZnO microflowers. For the degradation of Rhodamine B under visible light, the photocatalytic efficiency of ZnO/Cu2O submicrospheres reached 96% within 40?min of reaction time, which was 3.8 times higher than that of pure ZnO microflowers and up to 4.5 times than that for pure Cu2O nanoparticles. The remarkable visible light-driven photocatalytic performance is mainly attributed to the extended photoresponse range and effective separation of the photo-generated electron-hole pairs in the unique heterojunction.
Magnesium hydroxide and magnesium oxide nanostructures have been prepared by microwave/hydrothermal technique using magnesium metal in hydrogen peroxide (H2O2). The applied power of the microwave was 700?W for 10?min at 145?°C. The method produced Mg(OH)2 powder as a base material for MgO by calcinations at 550?°C for 2?h. X-ray diffraction data confirms the microwave production of Mg(OH)2 and (MgO) through the agreement with the standard JCDPS cards. Scanning electron microscopy shows nanoplates morphology for Mg(OH)2 and large-scale nanoplates with a hexagonal shape for MgO. The fundamental direct optical band gap of Mg(OH)2 equals 5.8?eV while for MgO equals 5.2?eV from the analysis of diffused reflectance data. MgO has higher dielectric constant than Mg(OH)2 at the higher frequencies. AC electrical conductivity increases with increasing the applied frequency for both materials. The microwave-hydrothermal technique shows a promising method for production of magnesium compounds from magnesium metal which can be used in different aspects such as catalysis, wastewater treatment, pharmaceutical and coated materials.
BaTiO3 (BTO) and BaTi1?xMnxO3 (x?=?0.25, 0.50, 0.75?mol%) ceramic materials have been prepared by the sol–gel combustion method. X-ray diffraction (XRD) has been carried out to characterize the phase purity and crystal structure of the prepared compounds, and all XRD patterns suggest tetragonal structure with the phase group of P4mm. The variation in the estimated lattice parameters confirms the incorporation of Mn atoms at Ti site of BTO. Raman spectroscopy studies under various temperatures suggest a phase transition from tetragonal to cubic phase at ~433?K, identified by a distinct Raman mode at 308?cm?1. As Raman modes are getting softened by Mn doping, phase transition temperature of the Mn-doped compounds is significantly decreased from 473?K (x?=?0%) to 433?K (x?=?0.75%). Dielectric properties such as permittivity and dielectric loss as the function of frequency under various temperatures have two distinct dielectric anomalies (i) at 393?K associated to tetragonal to cubic phase transition and (ii) at 550?K due to oxygen vacancy defect in the samples. Observation of weak ferromagnetism at 2, 300, and 400?K in the M (H) and ZFC-FC curve, suppose its origin due to an intriguing exchange interaction between Mn and oxygen vacancies.
Zinc gallate (ZnGa2O4) nanopowders doped with Cr3+ (1?mo%) were synthesized by the citric acid assisted sol–gel method. The influence of annealing temperature, structural, morphological, and optical properties of ZnGa2O4: Cr3+ (1?mol%) nanosized particles were investigated. The X-ray diffraction (XRD) spectra indicated that the nanoparticles are cubic in structure and the annealing temperature did not influence any c in structure. The average crystallite size of ZnGa2O4: Cr3+ nanoparticles were observed to increase from 11.85 to 30.88?nm as the annealing temperature increased from 600 to 1000?°C. The scanning electron microscopy (SEM) showed nearly spherical nanostructures that change in size with annealing temperature. The high resolution transmission electron microscope (HR-TEM) images show well resolved lattice fringes which is an indications of highly crystalline samples. Ultraviolet–visible (UV–Vis) measurement show decrease in reflectance in visible region and energy band gap was found to decrease with annealing temperature. The photoluminescence (PL) intensity was found to be maximum for sample annealed at high temperature (1000?°C) and least with sample annealed at low temperature (600?°C). An increase in annealing temperature leads significantly increment in PL intensity. The degree of crystallinity also increased with annealing temperature from XRD, SEM, and HR-TEM analysis. The photoluminescence lifetimes, particle size, and emission spectra are comparable with reports on bioimaging applications.
Nanocomposites of reduced graphene oxide (rGO) coupled gadolinium doped ZnFe2O4 (GZFG) have been successfully one pot in-situ synthesized adopting low temperature solution process from zinc nitrate, iron nitrate, gadolinium acetate and graphene oxide with varying concentrations of gadolinium (upto 10% Gd with respect to Zn) in the precursor medium. X-ray diffraction and transmission electron microscopy studies confirm the presence of single phase cubic spinel structure of ZnFe2O4 that uniformly distributed over the rGO layers. With increasing Gd doping concentration in precursor medium, the average crystallite size of ZnFe2O4 diminishes gradually from ~11 to ~5.5?nm. Raman and X-ray photoelectron spectral analyses confirm an existence of interaction between rGO and ZnFe2O4 in GZFG samples. Using antibiotic levofloxacin in water, the drug removal capacity (DRC) of GZFG has been performed by optimization of parameters such as gadolinium doping concentration in precursor medium, solution pH, etc. However, the gadolinium doping leads to an improvement in DRC of the nanocomposite and the 5% Gd doped sample shows about 86% DRC at the optimized condition. This simple strategy can be utilized in the synthesis of rGO coupled Gd doped other metal oxide nanocomposites for DRC application.
A new chemical approach for the fabrication of Fe3O4 embedded ZnO magnetic semicondutctor composite is reported. The method consists in increasing the pH of the synthesis solution by the thermal decomposition of urea instead of using common alkaline agents, such as NaOH and NH4OH. The material (Fe3O4@ZnO) was used as a platform for the fabrication of highly dispersed gold nanoparticles (~5?nm). The catalytic efficiency of the material, Fe3O4@ZnO@Au, was tested in the photodegradation of Rhodamine-B solutions, and prominent catalytic efficiency, stability, and recycling were achieved. A single portion of the catalyst could be used up to five times without significant loss of activity and its photodegradation efficiency was considered high even after the 12th cycle (56%). Catalyst separation after each batch could be easily achieved because of the intrinsic magnetic property of the material. Leaching monitoring of free Zn species during the fabrication of the catalyst suggests that the use of urea decreased substantially the formation of non-magnetic-semiconducting species and provided a higher mass yield of the magnetic composite compared to an analogous protocol using NaOH. The catalyst was also characterized by detailed structural and chemical analyses, such as transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and vibration sample magnetometer (VSM).
Superhydrophilic surfaces without the need of other stimuli are usually realized by constructing a rough morphology. However, constructing rough surfaces usually require specialized equipment or complicated processing. Besides, rough surfaces can cause undesirable scattering, which strongly limits the use in optical devices. In this article, we prepared superhydrophilic TiO2 films with ultra-smooth surfaces using simple sol-gel dip-coating method. The hydrophilicity of the TiO2 films varied with different post-heat treatments. The films heat-treated at 400?°C exhibited a durable superhydrophilicity and anti-fogging property. This superhydrophilicity was attributed to the decrease of surface hydrophobic alkoxy groups and the formation of point defects, i.e., Ti3+ and oxygen vacancies, which are favourable for dissociative water adsorption. The amount of surface organic groups was influenced by autophobicity effects, further hydrolysis and decomposition of residual alkoxy groups. Additionally, the wettability behaviours of the films were also explained from the perspective of the surface energy. These results can benefit the design and manufacture of anti-fogging and self-cleaning superhydrophilic TiO2 films.
Two series of TiO2 thin films were prepared based on soluble precursor powders: The first run originated directly from an alcohol-based coating solution whereas for the second batch the aqueous precursor powder sol had previously undergone a hydrothermal treatment. The respective microstructures were characterized by electron microscopy, the phase evolution was monitored by X-ray diffraction. Ellipsometric porosimetry (EP) was employed to reveal changes of porosity and pore size induced by thermal treatment of the films.
Soluble TiO2 precursor powders were hydrothermally treated to yield coating solutions. Films from these sols were compared with those directly obtained by dissolving the precursor powders. Results indicate that crystallization to anatase is induced under hydrothermal conditions and the resulting films mostly maintain their porosity throughout thermal treatment. In contrast to that coatings processed from as-dissolved precursor powders undergo more extensive densification
One of the promising candidates to replace the chromate conversion coatings for corrosion protection of aluminium alloy AA7075 are the hybrid sol–gel coatings. In the present work hybrid silica sol–gel coatings doped with cerium nitrate were prepared and characterized. Tetraethoxysilane (TEOS) and 3-glycidoxypropyl-trimethoxysilane (GPTMS) were used as precursors. Silica SiO2 (Ludox) particles were added to achieve a barrier properties of coating, while Ce(NO3)3·6H2O was added in order to obtain an active corrosion protection. Optimization of sol synthesis was based on the results of ATR-FTIR spectroscopy and UV–vis–NIR spectroscopy. Opening of epoxy rings and completion of hydrolysis and the condensation reactions during the synthesis process were confirmed. Coatings were characterized through thickness, water contact angle, roughness, adhesion, electrochemical properties (potentiodynamic and electrochemical impedance spectroscopy) and the response to prolonged immersion time in 0.1?M NaCl. The high degree of cross-linking of Si–O–Si network structure and high density was achieved during the synthesis of the sol. Moreover, the results showed that the curing process and the incorporation of cerium nitrate into the hybrid sol–gel coating affected to the corrosion properties of the coating. The observed enhancement in corrosion protection properties is attributed to the combination of the barrier properties of the silica matrix with the active protection of the cerium nitrate.
