Photocatalytic degradation of methylene blue with TiO2 nanoparticles prepared by a thermal decomposition process

The generation of TiO₂ nanoparticles by the thermal decomposition of titanium tetraisopropoxide (TTIP) was carried out experimentally using a tubular electric furnace at various synthesis temperatures (700-1300 °C) and TTIP heating temperatures (80-110 °C). The photocatalytic activity of the resulting TiO₂ nanoparticles was examined by measuring the rate of methylene blue decomposition. The TiO₂ nanoparticles were characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) measurements and transmission electron microscopy (TEM). The crystallite size and crystallinity increased with increasing synthesis temperature and TTIP heating temperature. A TTIP heating temperature and synthesis temperature of 95 °C and 900 °C, respectively, were found to be the optimal synthesis conditions. The primary particle diameter obtained under optimum synthesis conditions was considerably smaller than the commercial photocatalyst (Degussa, P25). The specific surface areas were more than 134.4 m² g^− 1. Under the optimal conditions, the photocatalytic activity for methylene blue was higher than that of the commercial photocatalyst.     

Preparation and characterization of 10 mol% Gd doped CeO2 (GDC) electrolyte for SOFC applications

Ceria-based materials are prospective electrolytes for low and intermediate temperature solid oxide fuel cells. In the present work, fully dense CeO₂ ceramics doped with 10 mol% gadolinium (Gd_0.1Ce_0.9O_1.95, GDC) have been prepared with a Pechini method. Characterization studies were realized with thermo-gravimetric analysis (TGA), differential thermal analysis (DTA), mass spectroscopy (MS), high temperature FT-IR (HT-FTIR) and X-ray diffraction analysis (XRD). A single-phase with a fluorite type structure was found to form at a relatively low calcination temperature of 500 °C. Dense GDC pellets having 98% of the relative density were obtained at sintering temperature of 1400 °C/6 h, which gave significantly higher total ionic conductivity of 3.4×10⁻² S cm⁻¹ at 500 °C in air. The present work showed that the Pechini method is a relatively low-temperature preparation technique to synthesize Gd_0.1Ce_0.9O_1.95 powders that provided high sinterability and good ionic conductivity.     

Physicochemical properties of ZnCl2-NaCl-KCl eutectic melt

Physicochemical properties of ZnCl₂-NaCl-KCl eutectic melt were studied at 200-300 °C for the first time. Firstly, it was reconfirmed that the eutectic composition is ZnCl₂:NaCl:KCl = 0.6:0.2:0.2 in mole fraction, and that the eutectic temperature is 203 °C. Then, the density, viscosity, and ionic conductivity of the ZnCl₂-NaCl-KCl eutectic melt were measured at 200-300 °C. At 250 °C, the density was 2.43 g cm⁻³, the viscosity was 42.0 cP and the ionic conductivity was 8.53 S m⁻¹. The temperature dependencies of density and ionic conductivity were well fitted by the VTF equations with the same ideal glass transition temperature of 283 K (10 °C). It was found that the melt obeys the fractional Walden's rule which is explained by the decoupling effect. The electrochemical window of the melt was determined to be 1.7 V at 250 °C with the cathode limit being zinc metal deposition and the anode limit being chlorine gas evolution.     

Nafion-TiO2 composite DMFC membranes: physico-chemical properties of the filler versus electrochemical performance

TiO₂ nanometric powders were prepared via a sol-gel procedure and calcined at various temperatures to obtain different surface and bulk properties. The calcined powders were used as fillers in composite Nafion membranes for application in high temperature direct methanol fuel cells (DMFCs). The powder physico-chemical properties were investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and pH measurements. The observed characteristics were correlated to the DMFC electrochemical behaviour. Analysis of the high temperature conductivity and DMFC performance reveals a significant influence of the surface characteristics of the ceramic oxide, such as oxygen functional groups and surface area, on the membrane electrochemical behaviour. A maximum DMFC power density of 350 mW cm⁻² was achieved under oxygen feed at 145 °C in a pressurized DMFC (2.5 bar, anode and cathode) equipped with TiO₂ nano-particles based composite membranes.     

Effect of Mg-and Fe-ions on formation mechanism of aluminium titanate

The presence of Mg²⁺- and Fe³⁺-ions has an effect on the formation of Al₂TiO₅. Crystalline phases produced under the influence of the heat treatment have been identified in a heated X-ray diffraction chamber in the temperature range of 20–1500 °C. In the presence of Mg²⁺- and Fe³⁺-ions transitional phases are formed in the temperature range of 1000–1350 °C during Al₂TiO₅ formation. The XRD technique was used to identify the crystalline phases formed. On addition of MgO, chemical composition of the transitional phase formed is Mg_0.3Al_1.4Ti_1.3O₅, whereas on addition of Fe₂O₃ we have calculated a Powder Diffraction File card data for the transitional phase. Determination of the lattice parameters of the Al₂TiO₅ ceramics produced enabled verification of incorporation of Mg²⁺- or Fe³⁺-ions into the crystal lattice of Al₂TiO₅, i.e. the formation of Mg²⁺- and Fe³⁺-containing solid solutions.     

Assessment of structurally stable cubic Bi12TiO20 as intermediate temperature solid oxide fuels electrolyte

Colloid processing and subsequent pressure filtration were used to prepare 14.3 mol% TiO₂ doped Bi₂O₃ (Bi₁₂TiO₂₀, 14BTO) as solid oxide fuel cell electrolyte. Materials characterization and electrical behaviors of 14BTO samples were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and two-point probe DC conductivity. A pure 14BTO with a cubic sillenite single phase was prepared at the sintering process of 850 °C with a high relative sintered density of 96.82%. In situ and batch-type long-term conductivity measurements at 600 °C were carried out to verify the possible reason of degradation. Additional reduction-oxidation tests under CH₄ atmosphere by thermogravimetric analysis (TGA) revealed possible application temperature of 14BTO electrolytes below 700 °C.     

Preparation of CuY catalyst using CuCl2 as precursor for vapor phase oxidative carbonylation of methanol to dimethyl carbonate

Cu^IY catalyst was prepared by heating the mixture of CuCl₂ and acidic Y zeolite under flowing nitrogen and characterized by TG/DTG, XRD and elementary analysis techniques. The experimental result indicate that when the heating temperature was from 350 °C to 500 °C, the CuCl₂ of the CuCl₂ and acidic Y zeolite mixture sample decompose to CuCl and Cl₂ gas, then the produced CuCl reacted with the Brønsted acid center H⁺ of Y zeolite to form Cu^IY catalyst by the solid-state ion-exchanged reaction. The amount of ion-exchanged Cu^I in the Cu^IY catalyst reached the maximum of 0.1 mol/g when the heating temperature was 650 °C, and the catalyst exhibited the best catalytic activity, the conversion of methanol (C_MeOH), the selectivity and the space-time yield of dimethyl carbonate (S_DMC and STY) reached 4.36%, 74.55% and 97.32 mg/(g h), respectively.     

Microstructure and ionic conductivity properties of gadolinia doped ceria (GdxCe1−xO2−x/2) electrolytes for intermediate temperature SOFCs prepared by the polyol method

Gd_0.1Ce_0.9O_1.95 and Gd_0.2Ce_0.8O_1.9 powders were prepared through the polyol process without using any protective agent. Microstructural and physical properties of the samples were characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetry (TG) and impedance analysis methods. The results of the thermogravimetry/differential thermal analysis (TG/DTA) and XRD indicated that a single-phase fluorite structure formed at the relatively low calcination temperature of 500 °C. The XRD patterns of the samples revealed that the crystallite size of the samples increased as calcination temperatures increased. The sintering behavior and ionic conductivity of pellets prepared from gadolinia doped ceria (GDC) powders, which were calcined at 500 °C, were also investigated. The relative densities of the pellets, which were sintered at temperatures above 1300 °C, were higher than 95%. The results of the impedance spectroscopy revealed that the GDC-20 sample that was sintered at 1400 °C exhibited an ionic conductivity of 3.25×10⁻² S cm⁻¹ at 800 °C in air. This result clearly indicates that GDC powder with adequate ionic conductivity can be prepared through the polyol process at low temperatures.     

Synthesis of a TiO2 ceramic membrane containing SrCo0.8Fe0.2O3 by the sol-gel method with a wet impregnation process for O2 and N2 permeation

A SrCo_0.8Fe_0.2O₃ impregnated TiO₂ membrane (TiO₂-SrCo_0.8Fe_0.2O₃ membrane) was successfully prepared using a sol-gel method in combination with a wet impregnation process. The membrane was subjected to a single gas permeance test using oxygen (O₂) and nitrogen (N₂). The TiO₂ membrane was immersed in the SrCo_0.8Fe_0.2O₃ solution, dried and then calcined to affix SrCo_0.8Fe_0.2O₃ into the membrane. The effect of the acid/alkoxide (H⁺/Ti⁴⁺) molar ratio of the TiO₂ sol on the TiO₂ phase transformation was investigated. The optimal molar ratio was found to be 0.5, which resulted in nanoparticles with a mean size of 5.30 nm after calcination at 400 °C. The effect of calcination temperature on the phase transformation of TiO₂ and SrCo_0.8Fe_0.2O₃ was investigated by varying the calcination temperature from 300 to 500 °C. X-ray diffraction spectroscopy (XRD) and Fourier transform infrared (FTIR) analysis confirmed that a calcination temperature of 400 °C was preferable for preparing a TiO₂-SrCo_0.8Fe_0.2O₃ membrane with fully crystallized anatase and SrCo_0.8Fe_0.2O₃ phases. The results also showed that polyvinyl alcohol (PVA) and hydroxypropyl cellulose (HPC) were completely removed. Field emission scanning electron microscopy (FESEM) analysis results showed that a crack-free and relatively dense TiO₂ membrane (∼0.75 μm thickness) was created with a multiple dip-coating process and calcination at 400 °C. The gas permeation results show that the TiO₂ and TiO₂-SrCo_0.8Fe_0.2O₃ membranes exhibited high permeances. The TiO₂-SrCo_0.8Fe_0.2O₃ membrane developed provided greater O₂/N₂ selectivity compared to the TiO₂ membrane alone.     

Preparation and magnetic properties of iron titanium oxide nanotube arrays

FeTi alloy was prepared by a vacuum smelting method, iron titanium oxide nanotube arrays have been made directly by anodization of the FeTi alloy. Morphologies and microstructures of the samples were characterized by scanning electron microscope, transmission electron microscope, and X-ray diffractometer. Influences of temperature and H₂O concentration on the morphologies of the nanotube arrays have been discussed in detail. Magnetic properties of the samples have also been investigated. The as-prepared samples were amorphous. When annealed at 500 °C and 550 °C, pesudobrookite Fe₂TiO₅ was obtained. At 600 °C, there were mixed Fe₂TiO₅, rutile TiO₂, and α-Fe₂O₃. Magnetic performance of the nanotube arrays exhibited high sensitivity to temperature and changed interestingly upon annealing. The values of the coercivity and remanence were 340 Oe and 0.061 emu/g respectively for the sample annealed at 550 °C.     

Low-temperature solution combustion synthesis of high performance LiNi0.5Mn1.5O4

High-voltage LiNi_0.5Mn_1.5O₄ spinels were synthesized by a low temperature solution combustion method at 400 °C, 600 °C and 800 °C for 3 h. The phase composition, structural disordering, micro-morphologies and electrochemical properties of the products were investigated by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM) and constant current charge–discharge test. XRD analysis indicated that single phase LiNi_0.5Mn_1.5O₄ powders with disordered Fd-3m structures were obtained by the method at 400 °C, 600 °C and 800 °C. The crystallinity increased with increasing preparation temperatures. XRD and FTIR data indicated that the degree of structural disordering in the product prepared at 800 °C was the largest and in the product prepared at 600 °C was the least. SEM investigation demonstrated that the particle size and the crystal perfection of the products were increased with increasing temperatures. The particles of the product prepared at 600 °C with ~200 nm in size are well developed and homogeneously distributed. Charge/discharge curves and cycling performance tests at different current density indicated that the product prepared at 600 °C had the largest specific capacity and the best cycling performance, due to its high purity, high crystallinity, small particle size as well as moderate amount of Mn³⁺ ions.     

Study on photoelectrochemical solar cells of nanocrystalline Cd0.7Zn0.3Se -water soluble conjugated polymer

Cadmium zinc selenide (Cd_0.7Zn_0.3Se) nanocrystalline thin films were chemically synthesized onto indium tin oxide (ITO)-coated glass substrate at relatively low temperature (<90 °C). The as-deposited films were annealed in air at 200, 300, and 400 °C for 60 min. The structure and surface morphology of the films were studied by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The water-soluble conjugated polymer, poly(2-ethynyl-N-carboxy-propyl-pyridinium bromide) (LM3), with quaternary pyridinium salts was layered by dipping the as-deposited and annealed Cd_0.7Zn_0.3Se films in the aqueous polymer solution. This hybrid photoanode system was subjected to photoelectrochemical (PEC) study under a light illumination intensity of 80 mW/cm².     

Comparison of the superconducting properties of Cu0.5Tl0.5Ba2Ca2(Cu3−yZny)O10−δ prepared at different synthesis temperatures

The superconducting properties of Zn-doped Cu_0.5Tl_0.5Ba₂Ca₂(Cu_3−yZn_y)O_10−δ {CuTlZn-1223} (y=0, 0.83, 1.66, 2.5) samples prepared at 820, 830, 850 and 860 °C have been compared. The samples were investigated by x-ray diffraction (XRD), dc-resistivity, ac-susceptibility and Fourier Transform Infrared (FTIR) absorption measurements. Almost all the superconducting properties have been increased to their maximum in all CuTlZn-1223 samples synthesized at 860 °C, which shows that 860 °C is the optimum temperature to achieve CuTlZn-1223 with enhanced superconducting properties.     

Correlation between sintering conditions and water contact angles for Ti–O thick films screen printed on an alumina substrate

TiO₂, TiO_2−x and Ti₃O₅ thick-film structures on corundum Al₂O₃ substrates were prepared using screen-printing technology. The screen-printed deposits were sintered up to 1500 °C in oxidising and reducing atmospheres to vary the Ti⁴⁺/Ti³⁺ ratio and consequently water contact angle. The structure of the thick films was studied with an X-ray powder diffractometer (XRD). The microstructural characteristics and the chemical composition were checked with a scanning electron microscope, equipped with an energy-dispersive spectrometer (EDS). The Ti–O films, up to 55 μm thick, exhibited excellent adhesion to the substrate and had uniform grain- and pore-size distributions. Ti₃O₅ and Al₂O₃ were found to be compatible phases up to 1500 °C in a reducing atmosphere. However, rutile-type TiO₂ and Al₂O₃ are not compatible compounds at temperatures up to 1400 °C, in either oxidising or reducing atmospheres. TiO₂ and TiO_2−x form two types of reaction products with Al₂O₃. These reaction products were found to have various Ti/Al ratios.     

Low-temperature synthesis of Bi2Fe4O9 nanoparticles via a hydrothermal method

Bi₂Fe₄O₉ (BFO) nanoparticles were successfully synthesized by a hydrothermal method at a temperature as low as 100 °C. The as-prepared powders, characterized by X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), transmission electron microscope (TEM) and physical property measurement system (PPMS), exhibited a pure BFO phase about 100 nm size with uniform sheet-like shape and exhibited an AF order at room temperature. It was found that high alkali concentration and alkali ion Na⁺ played a key role in the formation of BFO nanoparticles at a low temperature of 100 °C.     

Synthesis of La2NiO4 via a PVA-based route

Single-phase La₂NiO₄ has been prepared using polyvinyl alcohol (PVA) as a complexing agent. Thermogravimetric (TG), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) were used to characterize precursor and derived oxide powders. The particle size and morphologies of La₂NiO₄ crystallites were characterized by field emission scanning electron microscope (FSEM). The effect of the mol ratios of metal ion to hydroxyl groups in polyvinyl alcohol on the formation of La₂NiO₄ was investigated. XRD analysis showed that single-phase and well-crystallized La₂NiO₄ was obtained from precursor with M/OH = 1:3 at 900 °C. The La₂NiO₄ ceramics sintered at 1300 °C for 4 h exhibits an electrical conductivity of 42.5 Ω⁻¹ cm⁻¹ at room temperature.     

Effects of heating rate on microstructures and microwave dielectric properties of (1 − x)ZnAl2O4–xTiO2 (x = 0.21) ceramics

(1 − x)ZnAl₂O₄–xTiO₂ (x = 0.21) ceramics were synthesized at 1500 °C for 3 h using the solid-state reaction at a heating rate from 1 to 7 °C/min. The effects of heating rate on the microstructure, phase composition and oxidation state of titanium in the ceramics were investigated. The XRD results show that this system is composed of two phases, i.e. ZnAl₂O₄ spinel and rutile. The “black core” phenomenon resulting from reduction of Ti⁴⁺ ion valence appears after the ceramics are sintered at the speed of 1 and 3 °C/min. As the heating rate increases, the density and quality factor (Q·f) increase initially and reach the maximum value when the heating rate is 5 °C/min, and then reduce quickly to the minimum, while the dielectric constant (?_r) and temperature coefficient of resonator frequency (τ_f) nearly do not change. The optimal microwave dielectric properties can be achieved in (1 − x)ZnAl₂O₄–xTiO₂ (x = 0.21) ceramics sintered at a heating rate of 5 °C/min with an ?_r value of 11.6, a Q·f value of 74,000 GHz (at about 6.5 GHz), and a τ_f value of −0.4 ppm/°C.     

Onset coarsening-coalescence kinetics of ZrO2 and less refractory TiO2 nanoparticles: Effect of homologous temperature and phase transformation

Specific surface area change of ZrO₂ (predominant tetragonal - (t) symmetry, 30-50 nm) and less refractory TiO₂ anatase nanoparticles (20-50 nm) upon isothermal firing at 700-1000 °C in air was determined by N₂ adsorption-desorption hysteresis isotherm. The nanoparticles underwent onset coarsening-coalescence within minutes without appreciable phase transformation for TiO₂, but with extensive transformation into monoclinic (m-) symmetry for ZrO₂. The apparent activation energy of such a process being not much higher for ZrO₂ (77 ± 23 kJ/mol) than TiO₂ (56 ± 3 kJ/mol) nanoparticles can be attributed to transformation plasticity. The minimum temperature for coarsening/coalescence of the present ZrO₂ and TiO₂ nanoparticles was estimated as 710 and 641 °C, respectively.     

Improved performance of dense TiO2/CdSe coupled thin films by low temperature process

Dense TiO₂ and TiO₂/CdSe coupled nanocrystalline thin films were synthesized onto ITO coated glass substrate by chemical route at relatively low temperature (≤100 °C). TiO₂ films were nanocrystalline and crystallinity disappears after CdSe deposition as evidenced by X-ray powder diffraction. Surface morphology and physical appearance of films were studied from SEM and actual photo-images, reveals dense nature of TiO₂ (10-12 nm spherical grains, faint violet) and CdSe (80-90 nm spherical grains, deep brown), respectively. Presence of two absorption edges in UV spectra implies existence of separate phases rather than composite formation. TiO₂ film was found to have higher water contact angle (71°) than TiO₂/CdSe (61°) and CdSe (56°). I-V and stability tests of photo-electrochemical cells were performed with TiO₂ and TiO₂/CdSe film electrodes (under light of illumination intensity 80 mW/cm²) in lithium iodide as an electrolyte using two-electrode system.     

Synthesis of Bi0.5(Na0.7K0.2Li0.1)0.5TiO3 powders through the molten salt method

The Bi_0.5(Na_0.7K_0.2Li_0.1)_0.5TiO₃ powder synthesis through molten salt method was investigated in the temperature range of 650–700 °C for 2–4 h. The XRD results indicated that the optimal synthesizing temperature for molten salt method was 700 °C, significantly lower than that for conventional processing route of solid state reaction method, where a calcining temperature of 850 °C was needed. The SEM results revealed better crystallization of the powders obtained through molten salt method, compared with those through the conventional processing route of solid state reaction method.