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.
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.
A facile procedure was developed for the production of Al2O3 aerogels modified with tris(8-hydroxyquinolinato)aluminum complex (AlQ3). The addition of 8-hydroxyquinoline during the stage of alumina lyogel formation was found to increase gelation duration. The translucent monolithic aerogels were obtained by supercritical drying of lyogels in CO2. The composition and properties of aerogels were analyzed using low-temperature nitrogen adsorption, helium pycnometry, IR spectroscopy, UV–visible spectroscopy, luminescence spectroscopy, powder X-ray diffraction, scanning and transmission electron microscopy, and thermogravimetry combined with mass spectrometry. The obtained aerogels had low density (0.15–0.18?g?cm?3), high specific surface area (480–550?m2/g), high porosity (90–95%), and showed bright luminescence upon excitation in the UV range.
Powders of Sm0.6Sr0.4CoO3-δ and La0.6Sr0.4CoO3-δ were synthesized using wet chemical technique. Structural and surface properties of synthesized materials were studied by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), IR spectroscopy, and scanning electron microscopy (SEM). The influence of pH on the phase state, chemical composition, morphology, and fractal dimension of the synthesized powders were investigated. It was found that the change of pH has the influence on phase composition of synthesized powders. The increase of solution pH allows one to obtain homogeneous samples at lower temperatures down to 900–950?°C.
Barium zirconium titanate (Ba(ZrxTi1?x)O3, BZT) super smooth thin films are synthesized through modified sol-gel dip coating route on fluorine-doped tin oxide substrates with a suitably low calcination temperature. The Fourier tranformed infrared spectroscopy proves that impurities and starting materials are completely removed in the calcination process. Crystallographic phases of the samples are identified by the X-ray diffractometry and confirms that all samples are crystallized into a single perovskite phase. Introducing zirconium into the structure causes a reduction in dielectric constant of barium titanate. The optical properties of the films are also investigated. The results indicate that all samples are highly transparent and zirconium reduces the absorption coefficient. Moreover, the band gap energy of barium titanate increases when doped with zirconium and the highest band gap energy of about 3.71?eV along with the lowest dielectric constant of 850 at frequency of 100?kHz are obtained in 15 at.% zirconium-doped sample.
45S5 bioglass has been widely studied in the last few decades because of its bioactivity and promising applications in the biomedical field. Boron, even few studied, represents a potential element to improve the properties of the 45S5 bioglass derivatives. The bioglasses are conventionally prepared by heat treatment of oxides and silicon. Here, the sol?gel method is proposed for the preparation of the boron-based 45S5 bioglass (45S5B) and the classical 45S5 bioglass (45S5), using water-soluble salts as raw materials. The bioglasses were characterized by FTIR, XRD, and SEM, indicating the success of the sol?gel method for preparation of the samples. The bioglasses were also tested in vitro for bioactivity in biological conditions and cytotoxicity against eukaryotic cells. The bioactivity of 45S5B was similar to the bioactivity of 45S5 bioglass, indicated by the deposition of hydroxyapatite crystals at the surface of the pristine bioglasses. The results of cytotoxicity tests revealed that the IC50 of 45S5B (IC50?=?7.56?mg?mL?1) was similar to the IC50 of 45S5 (IC50?=?8.15?mg?mL?1), indicating its safety for application in the biomedical field.
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.
Thermally stable acid catalyzed mesoporous titania (TiO2) nanomatrices are obtained by sol–gel method for fiber optic pH sensing. These synthesized nanoparticles are annealed at 300?°C, at two time intervals i.e., 1?h and 2?h, characterized with several analytical techniques such as FE-SEM/EDS, AFM, XRD, FTIR, TGA, and Brunauer–Emmett–Teller (BET) analysis. Microscopic analysis shows that synthesized nanoparticles have crack-free, dense and homogeneous surface with low surface roughness (4.4–5.9?nm). EDS mapping confirms the uniform distribution of Ti in all samples. XRD findings revealed the TiO2 anatase phase. BET analysis shows that the mesoporous synthesized TiO2 nanoparticles have surface areas 169?m2/g and average pore diameter 39.2?Å. However, surface area is decreased to 113 and 102?m2/g and average pore diameter increased up to 62.36 and 68.18?Å after 1?h and 2?h heat treatment, respectively. Furthermore, the sensing activity of phenolphthalein (phph) doped mesoporous TiO2 nanoparticles/matrix is found to be high at pH 12 without any leaching/cracking.
Since the late 1960s, ceric hydrogen phosphates have attracted the attention of scientists due to remarkable ion exchange, sorption, proton-conduction and catalytic properties. In this work, through the application of various solvents, we, for the first time, have obtained monolithic aerogels based on ceric hydrogen phosphates with high porosity (~99%) and extremely low density (~10?μg/cm3). The composition and structure of aerogels were thoroughly studied with XRD, TEM, SEM, XPS, low temperature nitrogen adsorption methods, TGA/DSC, Fourier-transform infrared spectroscopy (FTIR) and small-angle neutron scattering (SANS). The aerogels were found to belong to the fibrous macroporous aerogels family.
A novel ZrCO composite aerogel is synthesized using zirconium oxychloride and resorcinol–formaldehyde (RF) as precursors through the sol–gel route and carbothermal reduction process. The effects of different Zr/R molar ratios and calcination temperatures on the physical chemistry properties of ZrCO aerogels are investigated. The ZrCO composite aerogel consists of the C/ZrO2/ZrC ternary aerogel. The results show that with the increase of R/Zr molar ratios, the specific surface area and bulk density increase with calcination temperature up to 1300?°C, but decrease at even temperature (1500?°C). The specific surface area is as high as 637.4?m2/g for ZrCO composite aerogel (R:Zr?=?2:1), which was higher than ever reported. As the heat-treatment temperature increases to 1500?°C, the ZrC crystalline phase occurs and the t-ZrO2 phase still appears within the composite. The thermal conductivity of the carbon fiber mat-reinforced composite aerogel is as low as 0.057?W/m/K at room temperature (25?°C).
Mixed-metal compounds, especially for the sulfides, have been investigated as a very attractive type of electroactive materials for supercapacitors. In this work, we demonstrate nickel?manganese (Ni?Mn) sulfides are very attractive for supercapacitors with promising electrochemical performance. The Ni?Mn sulfides with different Ni to Mn ratios have been synthesized via a facile one-pot hydrothermal method, which show a similar structure of interconnected particles and are very porous in microstructure. And then, the Ni?Mn sulfides are investigated by three-electrode measurements and demonstrate strong synergy between Ni and Mn. The Ni?Mn sulfide with a Ni to Mn ratio of 2:1 demonstrates superior performance of 1068?F?g?1 at 1?A?g?1. Lastly, The Ni?Mn sulfide with a Ni to Mn ratio of 2:1 are used as positive electrode for two-electrode test, and the asymmetric supercapacitor shows both high energy and power densities combined with excellent cycling stability. Our work demonstrates that the Ni?Mn sulfides are also very electrochemical active for supercapacitors and their performance can be tuned by changing the Ni to Mn ratio.
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.
The mesoporous silica samples with different concentrations of phosphonic acid groups on the surface were obtained by direct template synthesis. The block-copolymer Pluronic P123 was used as a template, and sodium meta-silicate with diethylphosphatoethyltriethoxysilane as precursors. According to the SAXS diffractograms, mesoporous silica samples have a p6mm hexagonal symmetry. In addition, we used sol–gel method to synthesize xerogel with the same groups for comparison. All samples possess high values of specific surface area 615–730?m2/g and sorption pore volume. FTIR and potentiometric titration methods were used to investigate the surface layer of these samples. Sorption properties of the samples with phosphonic acid groups were studied in respect to a row of metal cations, among which we focused on lead(II), cadmium(II), and dysprosium(III) cations.
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.
ZrC–ZrO2 composite ceramic microspheres were prepared by internal gelation combined with carbothermic reduction using fructose as a chelating agent and carbon source. Fructose in the precursor solution formed complex with zirconium ions, which was conducive to the refining of the microstructure of the sintered composite. ZrC–ZrO2 composite with ZrC content as high as 60?wt% could be prepared.
In this paper, fructose was used as a chelating agent and an organic carbon source to prepare ZrCO microspheres by internal gelation and carbothermic reduction. The fructose in the precursor solution could form complex with zirconium ions, which was conducive to the refining of the microstructure of the sintered composite. ZrC–ZrO2 composite with crystal size of ZrO2 and ZrC in nanometer range and ZrC content as high as 60?wt% could be successfully prepared.
The behaviour of alginate gel film in response to the tensile load is analysed in this paper. The bubbles of 0.5?mm diameter were embedded in the film by the fluidic method prior to gelation, thus providing uniform voidage over the entire film. Further, the intrinsic porosity of the gel matrix around the voids was varied by removing water through either evaporation under vacuum, or employing lyophilisation. The Poisson’s ratio and the modulus of elasticity were estimated from direct measurements. The viscoelasticity of the gel matrix was characterized from stress-relaxation measurement. The transient response to tensile loading and the evolution of stress contours were studied through numerical simulation in ANSYS. The ultimate strength was studied for the gel films with embedded voids of different sizes. The numerical simulations were validated by experimental measurements.
Fiber needle felt–silica aerogel composite was successfully prepared by via sol–gel process based on water glass. The thermal conductivity show V-type variation tendency with the increase of water to Si. Thermogravimetric analysis-differential scanning calorimetry analysis revealed that the thermal stability was up to approximately 390.58?°C. It has been found that the fire hazard of the composites decreased with the increased ratio of water to Si according to the cone calorimeter test, which can be characterized by peak heat release rate, fire performance index, and fire growth rate index. The fiber needle felt/aerogels present greatly improved compressive and flexural strength (elastic modulus: 0.1–0.97?MPa; flexural modulus: 0.33–0.66?MPa) while keeping inherent properties of pure silica aerogel: low bulk density (0.166?g/cm3), low thermal conductivity of 0.0236?W/m·K, and high specific surface area (1091.62?m2/g). As a result, the as-prepared composite shows a great potential to be applied in the thermal insulation field.
Brick-shaped zinc tungstate nanoparticles have been synthesized by ecofriendly solvent-free process using molten salts. Zinc tungstate nanobricks (ZnWO4 Nbs) were characterized by powder x-ray diffraction (PXRD), FTIR, Raman, energy dispersive and electron microscopic studies. ZnWO4 Nbs are used as the multifunctional electrode materials to oxygen generation reactions (OGR), oxygen reduction reactions (ORR) and supercapacitors (SCs) as well as photo-catalysts in the waste-water treatment by the degradation of organic dyes. Low overpotential (?10?=?0.475?V), low tafel slope (140?mV/dec), high current density (~70?mA/cm2) and good stability of the electrodes are the key results of the present studies for water electrolysis (OGR/ORR). ZnWO4 Nbs have also shown great interest in supercapacitors with efficient charge–discharge activities in 1?M KOH. The specific capacitance and energy density of ZnWO4 Nbs were found to be 250?F/g and 80?Wh/kg, respectively, at 5?mV/s, these values are relatively higher than that of previously reported specific capacitance and energy density value of metal tungstate nanoparticles. ZnWO4 Nbs as the photo-catalysts work very significantly for photocatalytic degradation of aqueous MB dye solution (~85 % in 3?h) in neutral medium.
ZnWO4 Nanobricks show significant multifunctional electro-chemical activities in alkaline medium and photocatalytic degradation of organic dye in neutral medium.
Rare earth element (i.e.) europium co-doped aluminum zinc oxide (Eu:AZO) thin films were deposited on microscope glass slides by nebulizer spray pyrolysis with different Eu-doping concentrations (0, 0.5, 1, and 1.5%). The deposited films were investigated using X-ray diffraction, AFM, EDAX, FT-Raman, UV–visible, PL, and Hall effect measurements. X-ray confirmed the incorporation of aluminum and europium ions into the ZnO structure. All films have polycrystalline nature with hexagonal wurtzite structure at (002) direction. Topological depictions exhibited minimum surface roughness and low film thickness for pristine AZO thin film. EDAX study authorizes the existence of Zn, O, Al, and Eu in Eu: AZO thin films. Raman spectra exhibited the characteristic of ZnO-wurtzite structure (E2-high) mode at 447?cm?1. The deposited film showed high optical transmittance of ~90% in visible region, and the direct energy gap was around 3.30?eV for pristine AZO thin film. The PL spectra emitted a powerful UV emission situated at 388?nm, and it indicates that the film has good optical quality. The obtained large carrier concentration and less resistivity values are 4.42?×?1021?cm?3 and 3.95?×?10?4?Ω?cm, respectively, for 1.5% Eu-doped AZO thin film. The calculated figure of merit value is 17.29?×?10?3 (Ω/sq)?1, which is more suitable for the optoelectronic device.
In this research, LiMn2O4 nanopowders were synthesized by the sol–gel method using gelatin as a chelating agent. Three categories of samples with various weight ratios of gelatin to the final product, 1:1, 2:1, and 3:1, have been synthesized. The produced gel was dried in a controllable oven with a slow slope up to 250??C and calcined at different temperatures. The results show that the amount of gelatin affects the structural properties such as the formation temperature of the spinel structure, the homogeneity of the size distribution and size of the particles. The sample with the weight ratio of 3:1 of gelatin to the final product has a lower temperature for the formation of LiMn2O4 with more homogeneity, and smaller particles with the average size of 70?nm, which is calcined at 750??C, while the samples with the weight ratios 2:1 and 1:1 have the average particle sizes of 75 and 89?nm, respectively.
