Structure and multiferroic properties of Bi<Subscript>5</Subscript>FeTi<Subscript>3</Subscript>O<Subscript>15</Subscript> thin films prepared by the sol–gel method

The Bi₅FeTi₃O₁₅ (BFTO) films of layered structure have been fabricated on Pt/Ti/SiO₂/Si substrates by the sol–gel method. The thermal decomposition behaviors of precursor powder were examined using thermo-gravimetric and differential scanning calorimeters analysis. The optimal heat treatment process for BFTO films were determined to be low-temperature drying at 200 °C for 4 min and high-temperature drying at 350 °C for 5 min followed by annealing at 740 °C for 60 min, which led to the formation of compact films with uniform grains of ~300 nm. The structural, surface topography, ferroelectric and magnetic properties of the films were investigated. The remnant polarization (2P _r) of BFTO thin films under an applied electric field of ~550 kV/cm are determined to be 67.5 μC/cm² . Meanwhile, the weak ferromagnetic properties of the BFTO films were observed at room temperature.     

Preparation and characterization of In<Subscript>2</Subscript>S<Subscript>3</Subscript> semiconductor thin films using the sol–gel method

This study describes the In₂S₃ semiconductor thin film coating on glass substrate by sol–gel method. The In₂S₃ thin film samples were prepared and examined by the X-ray diffraction (XRD), the UV–visible optical absorption and transmission study, and the Scanning Electron Microscope (SEM) image analyses. The XRD analysis results show that the In₂S₃ semiconductor thin films prepared by sol–gel method is formed at T~360–520 °C temperature interval. Band gap energy and optical absorption spectrum analysis of the In₂S₃ thin films reveal that Eg~2.51 eV for the In₂S₃ thin films. According to the EDX result the film was In-rich with the In/S = 1.42 ratio. The thickness of prepared In₂S₃ layer is about 400 nm.     

Synthesis and characterization of novel InVO<Subscript>4</Subscript>–TiO<Subscript>2</Subscript> thin films using the low temperature sol

The InVO₄ sol was obtained by a mild hydrothermal treatment (the precursor precipitation solution at 423 K, for 4 h). Novel visible-light activated photocatalytic InVO₄–TiO₂ thin films were synthesized through a sol–gel dipping method from the composite sol, which was obtained by mixing the low temperature InVO₄ sol and TiO₂ sol. The photocatalytic activities of the new InVO₄–TiO₂ thin films under visible light irradiation were investigated by the photocatalytic discoloration of methyl orange aqueous solution. The thin films were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and UV–Vis absorption spectroscopy (UV–Vis). The results revealed that the InVO₄ doped thin films enhanced the methyl orange degradation rate under visible light irradiation, 3.0 wt% InVO₄–TiO₂ thin films reaching 80.1% after irradiated for 15 h.     

Electrophoretic sol–gel synthesis of SrBi<Subscript>2</Subscript>Ta<Subscript>2</Subscript>O<Subscript>9</Subscript> nanowires

We report the independent invention of perovskite ferroelectric nanowires strontium bismuth tantalate (SrBi₂Ta₂O₉, SBT). Electrophoretic sol–gel techniques have been used successfully. The morphology and structures are analyzed via SEM, TEM and XRD. SBT nanowires and nanoparticles filled template revealed 30 and 40 μm long, respectively. SBT are proved to be a single phase of orthorhombic perovskite structure. As it indicated, SBT nanowires has been crystallized at 700 °C. To minimize surface polarity, SBT nanowires oriented preferentially along the growing axis (c axis) by translation and rotation of atomic clusters of SBT.     

Rietveld refinement of sol–gel Na<Subscript>2</Subscript>Ti<Subscript>6</Subscript>O<Subscript>13</Subscript> and its photocatalytic performance on the degradation of methylene blue

We have refined single crystals of Na₂Ti₆O₁₃ through the X-ray Rietveld method. The synthesis of the Na₂Ti₆O₁₃ was carried out by sol–gel method at 70 °C, and the obtained gel was heat treated at different temperatures. Through different analytical techniques such as X-ray Diffraction (XRD), Scanning Electronic Microscopy (SEM), Infrared Spectroscopy (FTIR), and Thermal Analysis (DTA/TGA), it was determined that Na₂Ti₆O₁₃ can be prepared at low temperature (750 °C) by sol–gel method. The product crystallizes in rectangular shape micro-fibers, free of impurities. Rietveld refinement was performed using X-ray diffraction technique taking as basis a monoclinic cell with space group C2/m. The following refined parameters were obtained: a = 15.095(7) Å, b = 3.745(3) Å, c = 9.174(1) Å, β = 99.01. Additionally, Na₂Ti₆O₁₃ was tested as photocatalysts on the degradation of methylene blue (MB) under UV light. The degradation reaction follows a first order reaction model with kinetic parameters k = 0.0089 min^?1, and t _1/2 = 78 min.     

Influences of synthesizing temperatures on the properties of Cu<Subscript>2</Subscript>ZnSnS<Subscript>4</Subscript> prepared by sol–gel spin-coated deposition

In this work Cu₂ZnSnS₄ (CZTS) suitable for the absorption layer in solar cells was successfully prepared by sol–gel spin-coated deposition. CZTS precursors were prepared by using solutions of copper (II) chloride, zinc (II) chloride, tin (IV) chloride, and thiourea. Texture structures with kesterite crystallinity reflected from the X-ray diffraction of (112), (200), and (312) planes of the CZTS were obtained as synthesized at a temperature of over 240 °C. The absorption coefficients of the CZTS films are higher than 10⁴ cm⁻¹, and the optical-energy gap is about 1.5 eV. Without sulfurization treatment, a near stoichiometry composition of the CZTS is obtained at a synthesizing temperature of 280 °C.     

B<Subscript>2</Subscript>O<Subscript>3</Subscript> additives on sintering and microwave dielectric behaviors of Mg<Subscript>4</Subscript>Nb<Subscript>2</Subscript>O<Subscript>9</Subscript> ceramics synthesized through the aqueous sol–gel Process

The relationships between the sintering temperatures and the microwave dielectric properties of (1−x)Mg₄Nb₂O₉-xB₂O₃ (x = 0.5–10 wt. %) compounds were investigated by the sol–gel method in order to reduce the sintering temperature in this study. A suitable amount of B₂O₃ doping was effective in allowing low sintering temperatures without a little detrimental effect on these dielectric properties of the Mg₄Nb₂O₉ compounds. The variations in the dielectric constant (ε _r ) and the quality factor (Q·f) of the Mg₄Nb₂O₉ compounds depended on the amount of B₂O₃ doping and the sintering temperature. As a result, a ε _r value of ~12.8 and a Q·f value of ~142,570 GHz were obtained when the Mg₄Nb₂O₉ compound with x = 3% was sintered at 1,200 °C for 4 h. The temperature coefficient of resonant frequency (τ _f ) of the 3%-B₂O₃ doping Mg₄Nb₂O₉ compound slightly changed from −33 to −48 ppm/°C with an increased sintering temperature.     

NiTiO<Subscript>3</Subscript> nanoparticles encapsulated with SiO<Subscript>2</Subscript> prepared by sol–gel method

NiTiO₃ (NTO) nanoparticles encapsulated with SiO₂ were prepared by the sol–gel method resulting on core-shell structure. Changes on isoelectric point as a function of silica were evaluated by means of zeta potential. The NTO nanoparticles heat treated at 600°C were characterized by X-ray diffraction, transmission electron microscopy (TEM) and energy dispersive X-ray analysis. TEM observations showed that the mean size of NTO is in the range of 2.5–42.5 nm while the thickness of SiO₂ shell attained 1.5–3.5 nm approximately.     

Rapid synthesis of the low thermal expansion phase of Al<Subscript>2</Subscript>Mo<Subscript>3</Subscript>O<Subscript>12</Subscript> via a sol–gel method using polyvinyl alcohol

Aluminum molybdate was successfully synthesized using a simplified PVA assisted sol–gel method resulting in highly crystalline, monophasic (monoclinic P2₁/a) samples. These materials could readily be obtained at temperatures of 600 and 700 °C after calcining for as little as 15–20 min. Scanning electron microscopy and X-ray powder diffraction indicated that even the sample calcined at 600 °C for 20 min was free of impurities and composed of submicron sized particles (~300 nm). Transmission electron microscopy was used to confirm the monophasic character and submicron dimensions of the as-prepared powders. In addition to producing high quality samples, it was also observed that the metal to PVA ratio used during this simplified synthesis, could be used as a control parameter for tailoring the particle sizes of the final product.     

Synthesis of Y<Subscript>3−x</Subscript>Lu<Subscript>x</Subscript>Al<Subscript>3</Subscript>MgSiO<Subscript>12</Subscript> garnet powders by sol–gel method

Y_3−xLu_xAl₃MgSiO₁₂ (x = 0–3) garnet powders were synthesized by an aqueous sol–gel method based on metal chelates with 1,2-ethanediol in aqueous media. Target samples were characterized by powder X-ray diffraction (XRD), scanning electron microscopy and reflection spectra. XRD analysis revealed that sintering of polycrystalline Y_3−xLu_xAl₃MgSiO₁₂ powders at 1,600 °C results in single-phase garnet materials.     

Preparation of Ga<Subscript>2</Subscript>Se<Subscript>3</Subscript> thin films by sol–gel technique

In this study we describe the preparation of Ga₂Se₃ semiconductor compound thin films by sol–gel method for different crystal formation temperatures. The films were characterized by X-ray diffraction analyses (XRD), UV–visible spectrometer, and scanning electron microscope (SEM). The XRD spectrum showed that the formation of Ga₂Se₃ crystals were between 743 and 823 K. The thin film crystals that were formed at 773 K corresponded to the β phase and the preferred crystal structure was monoclinic. The value of band gap from optical absorption spectra for the Ga₂Se₃ thin films was estimated to be about E _g ~ 2.56 eV. The thickness of the one-coat Ga₂Se₃ thin films, which was measured by a Spectroscopic Ellipsometer, was about ~200 nm. The average grain sizes of scattered particles were within the limits between 200 and 500 nm.     

Atmospheric control of gel-oxide transformation in sol–gel derived Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-Y<Subscript>2</Subscript>O<Subscript>3</Subscript> fibers

Via sol–gel processing metal–organic fibers were produced and dried up to 140 °C. For these gel fibers the influence of a treatment in different atmospheres was investigated for the temperature range of 200–850 °C. The atmospheres were nitrogen, water vapor, evaporated nitric and hydrochloric acid and evaporated hydrogen peroxide. In the presence of moisture and especially with acidic moisture fibers were transformed almost completely to their oxide composition (82 mol% Al₂O₃·18 mol% Y₂O₃). In these inorganic amorphous structures considerable differences were observed on several structural levels. On the atomic scale, the coordination of Al ions was investigated by ²⁷Al MAS NMR and skeletal density by He-pycnometry. Porosity in the nm scale was characterized by N₂-sorption. As a macroscopic effect of different treatment atmospheres, the longitudinal shrinkage was observed. For fibers treated at 500 °C the relative shrinkage varied by 100% (comparing water vapor and nitrogen atmosphere). No simple correlation between the release of organic constituents, the formation of porosity and the shrinkage could be found. These aspects were controlled by the rigidity of the inorganic network against atomic reconstitution. The kind of atmosphere was found to be an effective parameter to control various aspects of the xerogel structure.     

Preparation and characterization of Ba<Subscript>2</Subscript>Co<Subscript>2</Subscript>Fe<Subscript>12</Subscript>O<Subscript>22</Subscript> ferrite via glucose sol–gel method

Ba₂Co₂Fe₁₂O₂₂ (Co₂Y) was synthesized by sol–gel method using glucose as chelating agent. X-Ray diffraction studies indicate that sintering temperature as low as 950 °C is sufficient to produce Co₂Y ferrites. Co₂Y ferrites calcined at 1,000 °C exhibit good magnetic prosperities in high frequency, with the resonance frequency up to 11 GHz and intrinsic permeability about 5 even at 6 GHz. The heat-treated temperature dependence of coercivity, initial permeability and resonance frequency is close related to the particle shape and size.     

Synthesis and characterization of nanostructured Ba<Subscript>5</Subscript>Ta<Subscript>4</Subscript>O<Subscript>15</Subscript> by sol–gel process

Hexagonal Ba₅Ta₄O₁₅ were synthesized by a sol–gel process at temperatures of 700–900 °C. The microstructure properties and morphology are studied by X-ray diffraction and scanning electron microscope. Traces of the Ba₅Ta₄O₁₅ component were detected by energy dispersive X-ray analysis. A higher temperature enhanced higher atom mobility and caused the growth direction to change and created hexagonal square makes obvious good quality of samples. The visible light absorption edges of the Ba₅Ta₄O₁₅ nanorods and were corresponded to band-gap energies of 4.0 eV.     

A study on the effect of synthesis parameters on the size of nickel particles in sol–gel derived Ni–SiO<Subscript>2</Subscript>–Al<Subscript>2</Subscript>O<Subscript>3</Subscript> nanocomposites

The present work deals with the synthesis of Ni–SiO₂–Al₂O₃ nanocomposites fabricated by embedding nickel oxide particles, obtained from hexahydrated nickel nitrate [Ni(NO₃)₂ · 6H₂O], in matrixes with different molar percents of Silica/Alumina, through sol–gel method based on hydrolysis and condensation of tetraethylorthosilicate (TEOS) and Aluminum Isopropoxide [Al(OC₃H₇)₃] alkoxides. Due to the various factors, e.g., pH, EtOH/TEOS/H₂O ratio, Si/Ni ratio etc., influencing the nickel grain size of the nanocomposites, Taguchi robust design method of system optimization was used to determine the percent of contribution (%ρ) of each factor. The nanocomposites were reduced in a flow of hydrogen and nitrogen gas at 700 °C for half an hour. The nickel grain size in the nanocomposites was determined by utilizing Scherrer`s method and XRD patterns. The smallest nickel grain size obtained from the Taguchi orthogonal array was about 24 nm, later confirmed by TEM observations. After optimization of the controlling factors, a nickel grain size of 15.4 nm was obtained. It was found that the SiO₂/Al₂O₃ molar ratio of the matrix had the most influence on the nickel grain size (29.22%) and the Water/TEOS molar ratio stood in second place (21.44%). It was illustrated that the starting temperature of the aluminum isopropoxide had the least influence on the nickel grain size.     

Preparation of nanocrystalline CuAlO<Subscript>2</Subscript> through sol–gel route

Nanocrystalline powders of CuAlO₂ were synthesized through sol–gel method using nitrate-citrate route and also through solid state reaction method. We used a new set of precursor materials for the synthesis of CuAlO₂ through sol–gel route which were not reported in the past. A little lowering of the synthesis temperature (1,000 °C) was observed in case of sol–gel process compared to the solid state reaction method (1,100 °C) and also at shorter time duration. The particle size of the synthesized powders was determined through small angle X-ray scattering. It has been observed that the particle size prepared by nitrate-citrate technique is less than the particle size prepared by the solid-state reaction method. Chemical states of the atomic species were determined by X-ray photoelectron spectroscopy. The formation of phase pure CuAlO₂ were also confirmed by Fourier transformed infrared spectroscopy. A number of solvents were also used for finding the best possible combinations for obtaining phase pure CuAlO₂ at 1,000 °C and it was observed that only the combination of nitrate salts, citric acid and ethanol resulted phase pure CuAlO₂.     

B<Subscript>12</Subscript>-induced formation of stishovite in sol–gel produced amorphous SiO<Subscript>2</Subscript> matrices

Composites containing vitamin B₁₂ (cyanocobalamin) dispersed in amorphous silica xerogel were studied structurally as a function of annealing temperature. Silica xerogel samples were prepared by the sol–gel method using an ethanol:H₂O:TEOS molar ratio of 4:11.6:1 and loaded with cyanocobalamin. We found that the structure of the cobalamin is unaltered, although decoordination of the benzimidazole nucleobase of B₁₂, whereas the amorphous quartz structure of the matrix is maintained under heat-treatment without low-cristobalite phase transformation, typically of this kind of materials. We found in our samples partial crystallization of the glass matrix in form of stishovite obtained at very lower pressure than those specified by the phase diagram, and temperatures about 400 °C due to the presence of vitamin B₁₂. The presence of stishovite is corroborated by the Rietveld refinement method.     

Eu,Dy co-doped SrAl<Subscript>2</Subscript>O<Subscript>4</Subscript> phosphors prepared by sol–gel-combustion processing

SrAl₂O₄:Eu²⁺, Dy³⁺ powders were synthesized by sol–gel–combustion process using metal nitrates as the source of metal ions and citric acid as a chelating agent of metal ions. The amounts of citric acid in mole were two times those of the metal ions. By tracing the formation process of the sol–gel, it is found that decreasing the amount of NO₃ ⁻ in the solution is necessary for the formation of transparent sol and gel, and the dropping of ethanol into the precursor solution can decrease the amount of NO₃ ⁻ in the solution. By combusting citrate sol at 600 °C, followed by heating the resultant combustion ash at 1,100–1,300 °C in a weak reductive atmosphere containing active carbon, SrAl₂O₄:Eu²⁺, Dy³⁺ phosphors can prepared. X-ray diffraction, Thermogravimetry–differential thermal analysis, scanning electron microscopy and fluorescence spectrophotometer were used to investigate the formation process and luminescent properties of the as-synthesized SrAl₂O₄:Eu²⁺, Dy³⁺. The results reveal that the SrAl₂O₄ crystallizes completely when the combustion ash was sintered at 1,200–1,300 °C. The excitation and emission spectra indicate that excitation broadband mainly lies in a visible range and the phosphors emit strong light at 510 nm under the excitation of 348 nm. The afterglow of phosphors lasts for over 10 h when the excited source is cut off.     

Cu-particle-dispersed (K<Subscript>0.5</Subscript>Na<Subscript>0.5</Subscript>)NbO<Subscript>3</Subscript> composite thin films derived from sol–gel processing

Sol–gel processing of Cu-particle-dispersed (K_0.5Na_0.5)NbO₃ (Cu/KNN) thin films was studied in an attempt to develop a method producing piezoelectric composite films with good mechanical performance. The Cu/KNN films were prepared via crystallization annealing at 650–750 °C for 1 min in air, followed by reduction annealing at 400–500 °C for 1–2 h in a 5% H₂ and 95% Ar gas mixture. The resultant composite films consisted of perovskite KNN, metallic Cu, and Cu₄O₃. This suggests that the decomposition of Cu sources takes two different ways in this study. The Cu/KNN composite films containing Cu₄O₃ phases were produced by the crystallization annealing at 700 °C for 1 min followed by the reduction annealing at 500 °C for 1 h. Surface morphology observations reveal that these films have dense KNN matrix with a grain size of ~200 nm and uniformly dispersed Cu or Cu₄O₃ particles with a size of <500 nm.     

Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-based pigments synthesized by a new proteic sol–gel method

Alumina-based pigments were synthesized by the proteic sol–gel method. In this method, coconut water is employed as polymeric agent instead of the conventional alkoxide precursors. To this study, three common chromophore metallic ions (Mn³⁺, Co³⁺, and Cr³⁺) were chosen in order to verify the method efficiency. Differential thermal analysis (DTA), thermogravimetry (TG), and XRD techniques were used to characterize the synthesis process. The colorimetric characterization of the produced pigments was done according to the CIE-L*a*b* 1976 norm which is recommended by the CIE (International Commission on Illumination). The synthesized pigments presented intense and uniform colors in accordance to the literature results for each chromophore ion. The produced pigments also presented agglomerated with an average grain size of 180 nm when calcined at 800 °C.