Characterization and photoactivity of TiO2 sols prepared with triethylamine

Using triethylamine as a surface protective agent, a transparent and pale yellowish TiO₂ sol had been prepared at 90 °C. This method was very different from the traditional methods, which produced titanium dioxide nanoparticles with anatase crystalline structure either at high acid condition or high temperature. X-ray diffraction (XRD) and transmission electron spectroscopy (TEM) demonstrated that the as-prepared TiO₂ sol nanoparticles with anatase crystalline structure were uniformly distributed, and the average size was 3 nm. X-ray photoelectron spectroscopy (XPS) and UV-vis absorption spectra showed that triethylamine was adsorbed on TiO₂ sol particles surface. FTIR spectroscopy noted that TiO₂ sol particles had the similar spectra with Degussa P25. Photoactivity of the as-prepared TiO₂ sol was studied by investigating the photodegradation of methyl violet in hydrosol reaction system under visible light irradiation.     

Synthesis of nanostructured TiO2 particles in room temperature ionic liquid and its photocatalytic performance

Nanostructured TiO₂ particles were synthesized by sol-gel method with room temperature ionic liquid (RTIL) 1-n-butyl-3-methylimidazolium hexafluorophosphate ([BMIM][PF₆]) as a reaction medium. The structure and morphology of TiO₂ nanoparticles were characterized with X-ray powder diffraction (XRD) and transmission electron microscopy (TEM). The as-prepared TiO₂ nanoparticles present anatase crystal phase even without being calcined at high temperature, and show better photocatalytic performance in the degradation of methyl orange. The photocatalytic efficiency increases evidently along with increasing the concentration of nanostructure TiO₂, and the degradation percent can reach 100% at the optimal catalyst concentration (2.0 g/L).     

Synthesis and optical properties of TiO2 nanoparticles

Ultrafine TiO₂ particles have been synthesized successfully by a facile gas flame combustion method. The synthesized sample is characterized by X-ray diffraction (XRD), transmission electron micrograph (TEM), Fourier transform infrared (FTIR), and photoluminescence (PL) spectroscopy. The as-prepared TiO₂ nanoparticles appear to be a single anatase crystalline phase and the diameter is about 9 nm. Besides a sharp emission at 398 nm originating from the radiative annihilation of excitions, a weak broad band at about 434 nm from the defect-related emission is also discussed.     

The properties of Ba0.5Sr0.5TiO3 thin film prepared by RF magnetron sputtering from powder target

The Ba_0.5Sr_0.5TiO₃ (BST) thin film with the thickness of 400 nm deposited from powder target is prepared by the radio-frequency magnetron sputtering technique. The deposition rate of BST film is estimated to be 45 nm/min, which is very fast for ferroelectric materials. The dielectric properties of the as-prepared BST thin film are demonstrated. High dielectric tunability up to 42.7% and low dielectric loss small to 0.01 are achieved at a low applied voltage of 5 V. The results demonstrate that the RF magnetron sputtering from powder target is a versatile, novel technique for the deposition of high-quality ferroelectric thin films.     

Complexing reagent-assisted microwave synthesis of uniform and monodisperse disk-like CeF3 particles

Highly uniform and monodisperse disk-like CeF₃ particles with diameter about 230 nm and thickness about 76 nm were successfully synthesized via a mild and facile microwave irradiation assisted by a complexing reagent, ethylenediamine tetraacetic acid disodium salt (Na₂H₂EDTA). The morphologies and crystal structure of the products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and scanning electron microscopy (SEM). XRD patterns showed that the as-prepared CeF₃ products have hexagonal structure and high crystallinity. SEM images showed that these disk-like CeF₃ nanocrystals had rough surfaces which were covered with many sheet-like structures. It was found that the reaction time and the complexing reagent played crucial roles on formation of uniform disk-like CeF₃ particles. A possible formation mechanism of the disk-like CeF₃ particles was preliminarily presented.     

Rapid thermal melted TiO2 nano-particles into ZnO nano-rod and its application for dye sensitized solar cells

TiO₂ nano-particles with an anchored ZnO nano-rod structure were synthesized using the hydrothermal method to grow ZnO nano-rods and coated TiO₂ nano-particles on ZnO nano-rods using the rapid thermal annealing method on ITO conducting glass pre-coated with nano porous TiO₂ film. The XRD study showed that there was little difference in crystal composition for various types of TiO₂ nano-particles anchored to ZnO nano-rods. The as-prepared architecture was characterized using field-emission scanning electron microscopy (FE-SEM). Films with TiO₂ nano-particles anchored to ZnO nano-rods were used as electrode materials to fabricate dye sensitized solar cells (DSSCs). The best solar energy conversion efficiency of 2.397% was obtained by modified electrode material, under AM 1.5 illumination, achieved up to J_sc = 15.382 mA/cm², V_oc = 0.479 V and fill factor = 32.8%.     

Surfactant/co-polymer template hydrothermal synthesis of thermally stable, mesoporous TiO2 from TiOSO4

Industrial TiOSO₄ solution was used as inorganic precursor to prepare mesoporous titania via composite template route, using cetyl-trimethylammonium bromide (CTAB) and tri-block copolymer EO₂₀PO₇₀EO₂₀ (P-123) as structure-directing agents (SDA) under high acidic conditions. Mesoporous TiO₂ with high thermal stability was obtained via controlling the hydrolysis and condensation rate of industrial TiOSO₄ solution by adjusting the pH value and post hydrothermal treating. The as-prepared materials were characterized by XRD, nitrogen adsorption-desorption, SEM and HRTEM. The powder calcined at 723 K for 2 h showed higher thermal stability, with BET specific surface area of 218.7 m²/g and an average pore diameter of 3.63 nm.     

Nanocrystalline TiO2 thin films for NH3 monitoring: microstructural and physical characterization

Nanocrystalline titanium oxide thin films have been deposited by spin coating technique and then have been analyzed to test their application in NH₃ gas-sensing technology. In particular, spectrophotometric and conductivity measurements have been performed in order to determine the optical and electrical properties of titanium oxide thin films. The structure and the morphology of such material have been investigated by X ray diffraction, Scanning microscopy, high resolution electron microscopy and selected area electron diffraction. The X-ray diffraction measurements confirmed that the films grown by this technique have good crystalline tetragonal mixed anatase and rutile phase structure. The HRTEM image of TiO₂ thin film showed grains of about 50–60 nm in size with aggregation of 10–15 nm crystallites. Selected area electron diffraction pattern shows that the TiO₂ films exhibited tetragonal structure. The surface morphology (SEM) of the TiO₂ film showed that the nanoparticles are fine with an average grain size of about 50–60 nm. The optical band gap of TiO₂ film is 3.26 eV. Gas sensing properties showed that TiO₂ films were sensitive as well as fast in responding to NH₃. A high sensitivity for ammonia indicates that the TiO₂ films are selective for this gas.     

Photocatalytic properties of porous TiO2/Ag thin films

In this study, nanocrystalline TiO₂/Ag composite thin films were prepared by a sol-gel spin-coating technique. By introducing polystyrene (PS) spheres into the precursor solution, porous TiO₂/Ag thin films were prepared after calcination at a temperature of 500 °C for 4 h. Three different sizes (50, 200, and 400 nm) of PS spheres were used to prepare porous TiO₂ films. The as-prepared TiO₂ and TiO₂/Ag thin films were characterized by X-ray diffractometry (XRD) and by scanning electron microscopy to reveal structural and morphological differences. In addition, the photocatalytic properties of these films were investigated by degrading methylene blue under UV irradiation.When PS spheres of different sizes were introduced after calcination, the as-prepared TiO₂ films exhibited different porous structures. XRD results showed that all TiO₂/Ag films exhibited a major anatase phase. The photodegradation of porous TiO₂ thin films prepared with 200 nm PS spheres and doped with 1 mol% Ag exhibited the best photocatalytic efficiency where ∼ 100% methylene blue was decomposed within 8 h under UV exposure.     

Synthesis of monodisperse shuttle-like α-Fe2O3 nanorods via the EDA-assisted method

Monodisperse hematite shuttle-like nanorods were synthesized successfully by the ethylenediamine (EDA)-assisted method. The structure and morphology were investigated by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy dispersive X-ray spectrometer (EDS). XRD studies indicated that the as-prepared product was well-crystallized orthorhombic phase of α-Fe₂O₃. TEM and SEM images showed that the α-Fe₂O₃ nano-particles were of rod shape with an average length of 400 nm and diameter of about 80 nm in the middle part.     

Large-scale synthesis and characterization of fan-shaped rutile TiO2 nanostructures

Large-scale fan-shaped rutile TiO₂ nanostructures have been synthesized by means of a simple hydrothermal method using only TiCl₄ as titanium source and chloroform/water as solvents. The physicochemical features of the fan-shaped TiO₂ nanostructures are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), nitrogen absorption-desorption, diffuse reflectance ultraviolet-visible spectroscopy (UV-vis) and Fourier transform infrared spectroscopy (FTIR). Structural characterization indicates that the fan-shaped TiO₂ nanostructures are composed of several TiO₂ nanorods with diameters of about 5 nm and lengths of 300-350 nm. The average pore size and BET surface area of the fan-shaped TiO₂ nanostructures are 6.2 nm and 59 m²/g, respectively. Optical adsorption investigation shows that the fan-shaped TiO₂ nanostructures possess optical band gap energy of 3.11 eV.     

Co-emission of UV, violet and green photoluminescence of ZnO/TiO2 thin film

ZnO/TiO₂ thin films were fabricated on quartz glass substrates by E-beam evaporation. The structural and optical properties were investigated by X-ray diffraction (XRD), Raman spectra, optical transmittance and photoluminescence. XRD analysis indicates that the TiO₂ buffer layer can increase the preferential orientation along the (002) plane of the ZnO film. PL measurements suggest that co-emission of strong UV peak at 378 nm, violet peak at 423 nm and weak green luminescence at 544 nm is observed in the ZnO/TiO₂ thin film. The violet luminescence emission at 423 nm is attributed to the interface trap in the ZnO film grain boundaries.     

Ultrasonic spray pyrolysis of surface modified TiO2 nanoparticles with dopamine

Spherical, submicronic TiO₂ powder particles were prepared in the low temperature process of ultrasonic spray pyrolysis (150 °C) by using as a precursor aqueous colloidal solutions consisting of surface modified 45 Å TiO₂ nanoparticles with dopamine. Detailed structural and morphological characterization of colored submicronic TiO₂ spheres was performed by X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), laser particle size analysis and FTIR techniques. Also, optical characterization of both dopamine-modified TiO₂ precursor nanoparticles and submicronic TiO₂ powder particles was performed using absorption and diffuse reflectance spectroscopy, respectively. A significant decrease of the effective band gap (1.9 eV) in dopamine-modified TiO₂ nanoparticles compared to the band gap of bulk material (3.2 eV) was preserved after formation of submicronic TiO₂ powder particles in the process of ultrasonic spray pyrolysis under mild experimental conditions. Due to the nanostructured nature, surface-modified assemblage of TiO₂ nanoparticles preserved unique ability to absorb light through charge transfer complex by photoexcitation of the ligand-to-TiO₂ band, conventionally associated with extremely small TiO₂ nanoparticles (d < 20 nm) whose surface Ti atoms, owing to the large curvature, have penta-coordinate geometry.     

Hydrothermal synthesis of hemisphere-like F-doped anatase TiO<Subscript>2</Subscript> with visible light photocatalytic activity

Hemisphere-like F-doped anatase TiO₂ has been synthesized by hydrothermal treatment of TiF₄ aqueous solution in the presence of starch at 130 °C for 10 h, and then calcined at 450 °C for 2.5 h in air. The as-synthesized product has been investigated by photocatalytic reaction test and characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS), and UV–Vis diffuse reflectance spectra (DRS). The results showed that fluorine was successfully doped into the TiO₂ hemispheres. The F-doped TiO₂ hemispheres showed high visible light activity in degradation of acid orange II, which could be attributed to the creation of oxygen vacancies and good crystallinity.     

Preparation and characterization of N–I co-doped nanocrystal anatase TiO2 with enhanced photocatalytic activity under visible-light irradiation

N–I co-doped TiO₂ nanoparticles were prepared by hydrolysis method, using ammonia and iodic acid as the doping sources and Ti(OBu)₄ as the titanium source. The prepared catalysts were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and ultraviolet–visible diffuse reflection spectroscopy (UV–vis DRS). XRD spectra show that N–I–TiO₂ samples calcined at 673 K for 3 h are of anatase structure. XPS analysis of N–I–TiO₂samples indicates that some N atoms replace O atoms in TiO₂ lattice, and I exist in I⁷⁺, I⁻ and I⁵⁺ chemical states in the samples. UV–vis DRS results reveal that N–I–TiO₂ had significant optical absorption in the region of 400–600 nm. The photocatalytic activity of catalysts was evaluated by monitoring the photocatalytic degradation of methyl orange (MO). Compared with P25 and mono-doped TiO₂, N–I–TiO₂ powder shows higher photocatalytic activity under both visible-light (λ > 420 nm) and UV–vis light irradiation. Furthermore, N–I–TiO₂ also displays higher COD removal rate under UV–vis light irradiation.     

The effect of sputtering gas pressure on structure and photocatalytic properties of nanostructured titanium oxide self-cleaning thin film

Titanium oxide thin films were deposited by DC reactive magnetron sputtering on ZnO (80 nm thickness)/soda-lime glass and SiO₂ substrates at different gas pressures. The post annealing on the deposited films was performed at 400 °C in air atmosphere. The results of X-ray diffraction (XRD) showed that the films had anatase phase after annealing at 400 °C. The structure and morphology of deposited layers were evaluated by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The surface grain size and roughness of TiO₂ thin films after annealing were around 10-15 nm and 2-8 nm, respectively. The optical transmittance of the films was measured using ultraviolet-visible light (UV-vis) spectrophotometer and photocatalytic activities of the samples were evaluated by the degradation of Methylene Blue (MB) dye. Using ZnO thin film as buffer layer, the photocatalytic properties of TiO₂ films were improved.     

Synthesis and characterization of Co3O4 hollow spheres

Co₃O₄ hollow spheres were hydrothermally prepared at 130 °C for 16 h in the presence of Poly-vinylpyrrolidone (PVP). The as-prepared products were characterized by powder X-ray diffraction (XRD), field-emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM), infrared spectrum (IR), X-ray photoelectron spectrum (XPS), and optical absorption spectrum. PVP surfactant plays important roles in the formation of Co₃O₄ hollow spheres. These Co₃O₄ hollow spheres have average diameters of ca. 350 nm, and the wall thickness around the shell is about 42 nm. The possible formation mechanism of hollow Co₃O₄ spherical structures has simply been proposed.     

Preparation and characteristics of nanosized carbonated apatite by urea addition with coprecipitation method

Nanosized carbonated apatites (CAp) were prepared by coprecipitation method with urea addition at pH 8 and pH 12 with 12 hours aging, which resulted in needle-like and rod-like structures, respectively. From examining the XRD patterns, it was determined that the as-prepared powders contained no crystalline phase other than CAp. However, the powder prepared at pH 8 partially transforms to β-tricalcium phosphate (β-TCP) after heat treatment at 900 °C. Under heat treatment, powder prepared at pH 12 is more stable than powder prepared at pH 8. In addition, the as-prepared powders at pH 8 with 12 hours aging yield needle-like calcium deficient apatite (CDA) with substitution of CO₃^2? for PO₄^3? in low content. Their particle size is about 20 nm in width and 200–300 nm in length. The as-prepared powders at pH 12 for 12 hours aging result in rod-like nanostructures about 50 nm in diameter and 300 nm in length with 8.2 wt.% CO₃^2?, which is similar to human bone composition. Various characteristic analyses of CAp have been employed including X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), and transmission electron microscopy (TEM).     

Synthesis of GaN nanorods by ammoniating Ga2O3 films on TiO2 (rutile) layer deposited on Si(111) substrates

GaN nanorods have been synthesized by ammoniating Ga₂O₃ films on a TiO₂ middle layer deposited on Si(111) substrates. The products were characterized by X-Ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transformed infrared spectra (FTIR) and high-resolution transmission electron microscopy (HRTEM). The XRD analysis indicates that the crystallization of GaN film fabricated on TiO₂ middle layer is rather excellent. The FTIR, SEM and HRTEM demonstrate that these nanorods are hexagonal GaN and possess a rough morphology with a diameter ranging from 200 nm to 500 nm and a length less than 10 μm, the growth mechanism of crystalline GaN nanorods is discussed briefly.     

Microwave-assisted synthesis of ceria nanoparticles

Nanocrystalline ceria (CeO₂) particles have been successfully prepared by microwave-assisted heating technique from an aqueous solution containing ammonium Ce(IV) nitrate and sodium hydroxide. Further thermal treatment of the as-prepared powder at 500 °C resulted in the formation of the well-crystallized CeO₂ nanoparticles with an average crystal size of about 8 nm, varying with the heating temperature. The as-prepared powder and the CeO₂ nanoparticles were examined using X-ray diffraction (XRD) and transmission electron microscope (TEM) techniques. It was found that the morphologies of the synthesized powder show from rod-like for the as-prepared sample to sphere-like for the heat-treated nanoparticles. Mechanism of CeO₂ nanocrystallite growth during annealing is primarily investigated.