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Chemical modification of TiO2 by H2PO4−/HPO42− anions using the sol-gel route with controlled precipitation and hydrolysis: enhancing thermal stability

Abstract

Two titanium phosphate materials (TpP and ThP) have been successfully synthesized by sol-gel route with controlled precipitation and hydrolysis. The TpP material was obtained from the reaction between precipitated titania and phosphate buffer solution H2PO4− /HPO42− (pH = 7.3). The TpP material was prepared through hydrolysis of titanium in the presence of H2PO4−/HPO42. The probable state of the phosphate anions in titania framework and their effect on the anatase-to-rutile transformation were characterized by ICP-AES, DTA-TG, 31P NMR, FT-IR, and Raman analysis HRTEM/SEM. FT-IR and 31P NMR analyses of titanium phosphate TpP calcined at low temperature showed that the phosphate species existed not only as Ti-O-P in the bulk TiO2 but also as amorphous titanium phosphates, including bidentate Ti(HPO4)2 and monodentate Ti(H2PO4)4. Increased calcination temperature only gave an enrichment of bidentate structure on the titania surface. For the TpP material, H2PO4−/HPO42− anions were introduced into the initial solution, before precipitation, what promoted their lattice localization. At high temperatures, all the phosphorus inside the bulk of TiO2 migrated to the surface. The Raman analysis of both samples showed that the bidentate phosphates increased the temperature of the anatase-to-rutile phase transformation to more than 1000 °C with the formation of well crystalline TiP2O7 phase. This phenomenon was more evident for TpP sample.

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Microwave-assisted synthesis, characterization and photoluminescence of shuttle-like BaMoO4 microstructure

Abstract

Shuttle-like BaMoO4 microstructure has been successfully synthesized from Ba(N03)4H20 and Na2MoO2H2O as starting materials in ethylene glycol solvent containing 20 mL 5 M NaOH by microwave radiation at 180 W for 30 min. The as- synthesized BaMoO4 product was characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, Raman spectrophotometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and photolumines­cence (PL) spectroscopy. XRD patterns revealed that the products was tetragonal BaMoO4 phase. SEM and TEM characteriza­tion showed that the product had a shuttle-like BaMoO4 microstructure. PL of the shuttle-like BaMoO4 microstructure showed a maximum emission at 466 nm excited by 280 nm wavelength.

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Thermal and electrical properties of polyimide/PANI nanofiber composites prepared via in situ polymerization

Abstract

Polyimide/polyaniline nanofiber composites were prepared by in situ polymerization with various weight percentages of polyaniline (PANI) nanofibers. X-ray diffraction (XRD) and Fourier transform infrared spectra (FT-IR), proved the successful preparation of PANI nanofiber composite films. In addition, thermal stability of PI/PANI nanofiber composites was superior relative to PI, having 10 % gravimetric loss in the range of 623 °C to 671 °C and glass transition temperature of 289 °C to 297 °C. Furthermore, the values of the loss tangent tanδ and AC conductivity σAC of the nanocomposite films were notably higher than those of pure polyimide. The addition of 5 wt.% to 15 wt.% PANI nanofiber filler enhanced the activation energy of PI composites from 0.37 eV to 0.34 eV.

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Preparation of TiO2/Al-MCM-41 mesoporous materials from coal-series kaolin and photodegradation of methyl orange

Abstract

TiO2/Al-MCM-41 mesoporous materials were prepared via sol-gel method by loading titania onto Al-MCM-41 mesoporous molecular sieve by hydrothermal treatment from coal-series kaolin as raw material. The TiO2/Al-MCM-41 mesoporous materials were characterized by XRD, FT-IR, HRTEM, N2 adsorption-desorption and the photocatalytic degradation of methyl orange solution under visible light irradiation. The results showed that the TiO2/Al-MCM-41 mesoporous materials possessed a high surface area of 369.9–751.3 m2/g and a homogeneous pore diameters of 2.3–2.8 nm. The titania crystalline phase was anatase, and the particles size of TiO2 increased with TiO2 content. The Al-MCM-41 mesoporous materials exhibited excellent photodegradation activity under visible-light irradiation for methyl orange.

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Laser induced adjustment of the conductivity of rare earth doped Mn-Zn nanoferrite

Abstract

Two series of Mn-Zn nanoferrites (namely Mn1-xZnxFe2O4 and Mn1-xZnxFe2-yRyO4) were synthesized using standard ceramic technique. X-ray diffraction and FT-IR were employed in the chacterization of the nanopowder. The X-ray density for each sample increased after laser irradiation which was correlated with the decrease in the unit cell volume. The study involved the thermal and frequency variation of the dielectric constant and AC conductivity of the investigated samples before and after laser irradiation. The later altered the conductivity by decreasing its value for the rare earth doped samples except for the Sm3+ doped one. The results suggested the exploitation of Mn-Zn doped rare earth nanoferrites in many technological applications demanding high resistivity.

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Fabrication of Ag and Au nanoparticles in cross-linked polymer microgels for their comparative catalytic study

Abstract

Three dimensional cross-linked polymer microgels with temperature responsive N-isopropyl acrylamide (NIPAM) and pH sensitive methacrylic acid (MAA) were successfully synthesized by free radical emulsion polymerization with different amounts of MAA. Silver and gold nanoparticles with the size of 6.5 nm and 3.5 nm (±0.5 nm), respectively were homogeneously reduced inside these materials by chemical reduction method at pH 2.78 and 8.36 for the preparation of hybrid materials. The samples were characterized by FT-IR, DLS and TEM techniques. The catalytic activity of the hybrid materials was investigated for the reduction of 4-nitrophenol (4-NP) using NaBH4 as reducing agent by UV-Vis spectroscopy. The hybrid polymer network synthesized at pH 8.36 showed enhanced catalytic efficiency compared to the catalysts synthesized at pH 2.78. In this study, it has been stated that the catalyst activity strongly depends on the amount of MAA, pH value during synthesis and the type of entrapped metal nanoparticles.

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TiO2 supported on SiO2 photocatalysts prepared using ultrasonic-assisted sol-gel method

Abstract

TiO2-SiO2 (TiO2 supported on SiO2) photocatalysts were prepared using an ultrasonic-assisted sol-gel method. These photocatalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and photoluminescence spectra (PL). Their photocatalytic activities were investigated by the method of methyl orange oxidation. It was found that the photocatalytic activity of TiO2-SiO2 was optimal when the molar ratio of hexadecyl trimethyl ammonium bromide to titanium butoxide was 1:10. The average crystallite size of TiO2-SiO2 was smaller than that prepared by the stirring method. Furthermore, for pure anatase phase samples, it was shown that the lower the photoluminescence intensity, the higher the photocatalytic activity.

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Preparation and dielectric properties of BaBi1.8Ln0.2Nb2O9 (Ln = Ce, Gd) ceramics

Abstract

The main subject of the presented research is to investigate the dielectric properties of BaBi1.8Ln0.2Nb2O9 (Ln = Ce, Gd) ceramics prepared by conventional solid state reaction route. The materials were examined using XRD and FT-IR methods. Moreover, the AC conductivity, dielectric constant and dielectric loss of the ceramics were determined. X-ray diffraction confirmed that all these compounds crystallize in an orthorhombic structure. Fourier transform infrared spectroscopy study confirmed the presence of two characteristic vibration bands located at around 617 cm-1 and 818 cm-1 for BaBi2Nb2O9. The experimental results show that the substitution of Bi by Ce or Gd causes a decrease in Curie temperature, dielectric constant and dielectric loss.

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Facile Synthesis of Spinel Nanocrystalline ZnFe2O4: Enhanced Photocatalytic and Microbial Applications

Abstract

Spinel ZnFe2O4 was developed successfully as a heterogeneous-Fenton catalyst for the degradation of Reactive Yellow 86 (RY 86) under UV light. The ZnFe2O4 was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM) and UV-diffuse reflectance spectroscopy (UV-DRS). FE-SEM reveals that the some of the particles sizes are in the range from 10 nm to 50 nm. The photocatalytic performance of ZnFe2O4 was evaluated by degradation of RY 86 dye solution under UV light. The degradation rate was highly influenced by pH, initial concentrations of H2O2 and catalyst concentration. The results indicated that ZnFe2O4 could be used as a photocatalyst for treatment of industrial coloured wastewater. The catalyst was reused for five consecutive runs without significant change in its activity. Moreover, the antibacterial effects were investigated.

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Growth, solvent effect, optical and electrical properties of sodium 4-hydroxybenzenesulfonate dihydrate

Abstract

Single crystal of sodium 4-hydroxybenzenesulfonate dihydrate (Na-4-HBS) was grown from an aqueous solution by slow evaporation method. Powder X-ray diffraction study was carried out to identify the lattice parameters of the crystal. FT-IR spectral analysis confirmed the existence of various functional groups in the compound. The optical transmittance, cut-off wavelength and band gap energy were estimated from the UV-Vis studies. Photoluminescence studies revealed the transition mechanism by optical excitation. The variation of dielectric properties and AC conductivity of the grown crystal with frequency was studied at different temperatures. Measurements of mechanical properties of Na-4-HBS were carried out to find the hardness of the material. The laser induced surface damage threshold and relative second harmonic generation nonlinear optical properties of the grown crystal were studied using Q-switched Nd:YAG laser.

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