Fine-sized BaMgAl10O17:Eu phosphor powders prepared by spray pyrolysis from the spray solution with BaF2 flux

Fine-sized BaMgAl₁₀O₁₇:Eu²⁺ phosphor powders with plate-like morphology were prepared by spray pyrolysis process. The effects of ratio of BaF₂ and Ba(NO₃)₂ used as the source materials of Ba component on the morphological and optical properties of the BaMgAl₁₀O₁₇:Eu²⁺ phosphor powders were investigated. BaF₂ was used as the flux material as well as the source material of Ba component. The phosphor powders prepared from the spray solution with the same mole concentrations of BaF₂ and Ba(NO₃)₂ had fine size, plate-like morphology and narrow size distribution. The addition of BaF₂ as the source material of Ba component increased the photoluminescence intensities of the phosphor powders. The phosphor powders prepared from the spray solution with the ratios of BaF₂ and Ba(NO₃)₂ larger than 1 had the similar photoluminescence intensities to that of the commercial product.     

Non-isothermal crystallization kinetics of nano-sized amorphous TiO2 prepared by facile sonochemical hydrolysis route

The synthesized nano-sized amorphous TiO₂ was successfully obtained by sonochemical hydrolysis of titanium tetraisopropoxide (TTIP). The microstructure and amorphous feature of TiO₂ were examined by X-ray diffraction (XRD) as well as high-resolution transmission electron microscope (HRTEM). Moreover, the selected area electron diffraction (SAED) pattern confirmed the amorphous nature of the obtained titania (TiO₂) powder. The thermal behavior of the obtained titania powder was studied using differential scanning calorimetry (DSC) measurements and thermogravimetry (TG) analysis. The transformation characterization of amorphous to anatase titania phase was carried out using the obtained exothermic peaks for anatase crystallization under the investigated non-isothermal conditions of the DSC measurements at constant heating rates (5, 10, 15 and 20?°C/min). The investigated transformation of amorphous to anatase titania was introduced using model-free isoconversional approach. The crystallization kinetics together with its dimensionality were studied to identify the growth of the anatase phase. The obtained results showed the independency of the activation energy of crystallization on the crystallized fraction and it has been found around 202.4?±?7.5 $\mathrm{KJ}/\mathrm{mol}$. Moreover, the dimensionality of crystal growth found to be in one direction that is identifying the crystallization process by dominated nucleation is the surface nucleation. The growth mechanism was discussed in view of the expected homogeneous formation of a large number of seed nuclei during sonochemical reaction.     

Developing the properties of new blue phosphors: TiO2-doped Zn2SiO4

2ZnO + SiO₂ + X mol% TiO₂ (Zn₂SiO₄-X-TiO₂, 1 ≤ X ≤ 3) and 2ZnO + SiO₂ + 3 mol% MnO₂ (Zn₂SiO₄-3-TiO₂) compositions were prepared using nanoscale ZnO, SiO₂, TiO₂, and MnO₂ particles. The mixing powders were calcined between 1000 °C and 1300 °C in a N₂ atmosphere. Zn₂SiO₄ was the only phase in the calcined Zn₂SiO₄-X-TiO₂ phosphors. We found that the photoluminescence (PL) properties of synthesized Zn₂SiO₄-X-TiO₂ phosphors revealed these to be blue rather than green. The effects of TiO₂ content and calcining temperature on the PL properties of Zn₂SiO₄-X-TiO₂ phosphors were rigorously investigated.     

Fabrication and properties of highly transparent Tm3Al5O12 (TmAG) ceramics

Highly transparent Tm₃Al₅O₁₂ (TmAG) ceramics were fabricated by solid-state reaction and vacuum sintering. Densification, microstructure evolution, mechanical, thermal, and optical properties of the TmAG ceramics were investigated. Fully dense TmAG ceramic with average grain size of 15 μm was obtained by sintering at 1780 °C for 20 h. The in-line transmittance was 80.5% at 2000 nm. The absorption coefficients at 682 nm and 785 nm were 8.03 cm⁻¹ and 8.33 cm⁻¹, respectively. The Vickers hardness, the Young modulus, the bending strength, and the fracture toughness values were 15.14 GPa, 343 GPa, 230 MPa, and 2.35 MPa m^1/2, respectively. The thermal conductivity at room temperature was 3.3 W/m K and the average linear thermal expansion coefficient from 20 °C to 1000 °C was 8.915 × 10⁻⁶ K.     

The characteristics of X1 type Y2SiO5:Tb phosphor particles prepared by high temperature spray pyrolysis

The X1 type Y₂SiO₅:Tb phosphor particles with high brightness were prepared by spray pyrolysis from spray solution with NH₄F flux material. The phosphor particles prepared by spray pyrolysis at high preparation temperature had spherical shape, fine size and dense morphology. The mean sizes of the phosphor particles prepared at 900 and 1650 °C were 1.3 and 0.9 μm. The emission spectrum of the phosphor particles prepared by spray pyrolysis at 1650^oC had the characteristics of X1 type Y₂SiO₅:Tb phosphor. The photoluminescence intensity of the phosphor particles directly prepared by spray pyrolysis from spray solution with 20 wt.% NH₄F flux of the product at temperature of 1650 °C was 127 and 184% of the X1 and X2 type Y₂SiO₅:Tb phosphor particles post-treated at 1100 and 1300 °C, respectively. The Y₂SiO₅:Tb phosphor particles prepared by spray pyrolysis at 1650 °C had X1 type crystal structure because of short residence time of particles inside hot wall reactor of 0.4 s.     

Synthesis of nano-sized Yb3Al5O12 powders by the urea co-precipitation method

Nano-sized polycrystalline ytterbium aluminum garnet (YbAG, Yb₃Al₅O₁₂) powders were successfully synthesized by a simple urea co-precipitation method. The thermal behavior of the YbAG precursor was investigated. The calcined amorphous YbAG precursor was directly converted to 20–30 nm monophase YbAG at as low as temperature 900 °C, without any other intermediate phases. The nano-sized YbAG powders calcined at 900 °C distributed evenly with a slight aggregation, and the specific surface area of the powders reached 29.7 m² g⁻¹. The absorption spectrum of the YbAG powders was measured, and there were two strong absorption peaks centered at 931 and 965 nm. The results did not correspond to the absorption peaks of Yb:YAG crystal exactly, as the lattice parameters were different between YbAG and YAG.     

Thermal conductivity of AlN ceramics sintered with CaF2 and YF3

Dense AlN ceramics with a thermal conductivity of 180W/m·K were obtained at the sintering temperature of 1750 °C using CaF₂ and YF₃ as additives. At temperatures below 1650 °C, the shrinkage of AlN ceramics is promoted by liquid (Ca,Y)F₂ and Ca₁₂Al₁₄O₃₂F₂. Liquid CaYAlO₄ mainly improves the densification of the sample when the sintering temperature increases to 1750 °C. The formation of liquid (Ca,Y)F₂ at a relatively low temperature results in homogeneous YF₃ distribution around the AlN particles, which benefits the removal of oxygen impurity in the AlN lattice, and thus a higher thermal conductivity.     

Hot-pressing sintered BN-SiO2 composite ceramics with excellent thermal conductivity and dielectric properties for high frequency substrate

High thermal conductivity and low dielectric constant are the more and more important properties for high-frequency substrate materials to enhance their heat radiation and reduce signal delay. In this work, a series of BN-SiO₂ composite ceramics for high frequency application were successfully synthesized by hot-pressing sintering method. And their structures, thermal and dielectric properties were systematically studied. According to the results, the excellent thermal conductivity with low dielectric constant and low dielectric loss has been obtained in the BN-SiO₂ ceramic. Compared to the pure SiO₂, the sample with 50?wt% BN addition sintered at 1650?℃ exhibited excellent physical properties, including a high thermal conductivity of 6.75?W/m?K which is almost five times higher than that of pure SiO₂ and a low dielectric constant of 3.73. The achieved high thermal conductivity and appropriate dielectric property of the BN-SiO₂ composite ceramic make it a promising candidate for high-frequency substrate application.     

Spectroscopic ellipsometry characterization of TiO2 thin films prepared by the sol–gel method

TiO₂ thin films were prepared on SiO₂/Si(100) substrates by the sol–gel process. XRD results indicate that the major phase of TiO₂ thin films is anatase. The surface morphology and cross-section are observed by FE-SEM. The surface of thin films is dense, free of cracks and flat. The average grain size is about 60–100 nm in diameter. The thickness of single layer TiO₂ thin films is about 60 nm, which increases with the concentration of solution. Ellipsometric angles ψ, Δ are investigated by spectroscopic ellipsometry. The optical constant and the thickness of TiO₂ thin films are fitted according to Cauchy dispersion model. The results reveal that the refractive index and the extinction coefficient of TiO₂ thin films in wavelength above 800 nm are about 2.09–2.20 and 0.026, respectively. The influences of processing conditions on the optical constants and thicknesses of TiO₂ thin films are also discussed.     

Electrical properties of (Bi2O3)0.75(RE2O3)0.25 ceramics (RE=Dy, Y, Ho, Er and Yb)

Five kinds of rare earth stabilized bismuth oxide ceramics, (Bi₂O₃)_0.75(RE₂O₃)_0.25 (RE=Dy, Y, Ho, Er and Yb), were synthesized by sintering a mixture of Bi₂O₃ and RE₂O₃ at 900–1100 °C and their electrical properties were investigated. The bulk density and the lattice constant linearly increased with an increase in the atomic weight of RE and the ionic radius of RE³⁺, respectively. The electrical conductivity at 300 °C slightly increased with the increasing ionic radius of RE³⁺, while at 500 and 700 °C, it was constant regardless of the ionic radius of RE³⁺. The migration activation energy and the association activation energy showed a maximum value and a minimum value at RE=Er, respectively.     

Spontaneously ordered TiO2 nanostructures

Titanium dioxide thin films were deposited on quartz substrates kept at different O₂ pressures using pulsed laser deposition technique. The effects of reactive atmosphere and annealing temperature on the structural, morphological, electrical and optical properties of the films are discussed. Growth of films with morphology consisting of spontaneously ordered nanostructures is reported. The films growth under an oxygen partial pressure of 3 × 10⁻⁴ Pa consist in nanoislands with voids in between them whereas the film growth under an oxygen partial pressure of 1 × 10⁻⁴ Pa, after having being subjected to annealing at 500 °C, consists in nanosized elongated grains uniformly distributed all over the surface. The growth of nanocrystallites with the increase in annealing temperature is explained on the basis of the critical nuclei-size model.     

Low temperature mechanical behavior of 1D-Cf/SiO2 composite

Unidirectional carbon fiber reinforced fused silica (1D-C_f/SiO₂) composite was prepared by slurry infiltration and hot-pressing. The flexural strength and the coefficient of thermal expansion (CTE) at room and liquid nitrogen temperature (77 K) were investigated. The flexural strength of the composite tested at 77 K was 878 MPa, higher than that 667 MPa at room temperature. Moreover, the CTE of the composite at 77 K was higher than that at room temperature. Due to the difference of CTE between the matrix and fiber, gaps appeared at the fiber/matrix interface of as-prepared specimens. However, they may be healed up because of the thermal expansion of carbon fiber at 77 K. It led to a higher interfacial sliding resistance and changed the weak fiber/matrix interfacial bonding. Thus, it was helpful for the load transfer from matrix to fiber.     

Isothermal crystallization kinetics and effect of crystallinity on the optical properties of nanosized CeO2 powder

The isothermal crystallization kinetics and effect of crystallinity on the optical properties of cerium dioxide (CeO₂) nanopowders synthesized using a coprecipitation route at 293 K and pH 9 were investigated using X-ray diffraction, transmission electron microscopy, selected area electron diffraction, and ultraviolet–visible absorption spectrophotometry. The activation energy of CeO₂ crystallization from dried cerium dioxide precursor powders by isothermal method of 64.1±3.24 kJ/mol was obtained. The average value of the growth morphology parameter (n) is 1.94, meaning that two-dimensional growth with plate-like morphology was the primary mechanism of CeO₂ crystallization from cerium dioxide precursor powders. The indirect band gap energy (E_i) of CeO₂ decreased from 3.03 eV to 2.83 eV when the crystallinity increased from 18% to 82%, and the direct band gap energy (E_d) of CeO₂ also decreased from 3.76 eV to 3.64 eV.     

VUV photoluminescence properties of Y1−xGdxVO4:Eu phosphors prepared by ultrasonic spray pyrolysis

The red-emitting (Y_1−xGd_x)_0.94Eu_0.06VO₄ (0 ≤ x ≤ 1.0) phosphors were synthesized by ultrasonic spray pyrolysis. The (Y_1−xGd_x)_0.94Eu_0.06VO₄ (0 ≤ x ≤ 1.0) phosphors had the tetragonal xenotime structure with a space group of I4₁/amd (1 4 1). The calculated crystallite sizes of the annealed phosphors ranged from 58 to 68 nm. In this study, we discussed the photoluminescence properties of the (Y_1−xGd_x)_0.94Eu_0.06VO₄ phosphors under VUV excitation, depending on Gd content. The emission intensity of the (Y_1−xGd_x)_0.94Eu_0.06VO₄ phosphors increased with increasing Gd content up to x = 0.5, and then decreased with a further increase in Gd content. The purest red color was obtained for the (Y_0.5Gd_0.5)_0.94Eu_0.06VO₄ phosphors.     

Hydrophilic/hydrophobic conversion of Ni-doped TiO2 thin films on glass substrates

Nickel-doped titanium oxide thin films were prepared on soda–lime–silica glass substrates by using a metal naphthenate. Films prefired at 500 °C for 10 min were finally annealed at 600 °C for 30 min in air. Contact angle measurement was used for analyzing hydrophilic/hydrophobic conversion. NiTiO₃, rutile and anatase peaks were obtained for the film after nickel doping. The film containing nickel showed a shift towards the visible in the absorption threshold.     

TiO2, TiO2/Ag and TiO2/Au photocatalysts prepared by spray pyrolysis

TiO₂, TiO₂/Ag and TiO₂/Au photocatalysts exhibiting a hollow spherical morphology were prepared by spray pyrolysis of aqueous solutions of titanium citrate complex and titanium oxalate precursors in one-step. Effects of precursor concentration and spray pyrolysis temperature were investigated. By subsequent heat treatment, photocatalysts with phase compositions from 10 to 100% rutile and crystallite sizes from 12 to 120 nm were obtained. A correlation between precursor concentration and size of the hollow spherical agglomerates obtained during spray pyrolysis was established. The anatase to rutile transformation was enhanced with metal incorporations and increased precursor concentration. The photocatalytic activity was evaluated by oxidation of methylene blue under UV-irradiation. As-prepared TiO₂ particles with large amounts of amorphous phase and organic residuals showed similar photocatalytic activity as the commercial Degussa P25. The metal incorporated samples showed comparable photocatalytic activity to the pure TiO₂ photocatalysts.     

Optical and ferromagnetic properties of hydrothermally synthesized CeO2/CuO nanocomposites

Nanostructured CeO₂/CuO composites are synthesized using a facile hydrothermal reaction. Results signify that Cu ions prefer to enter into CeO₂ lattice forming solid solution at low concentration, and would be transformed into CuO phase at moderate concentration. Moreover, the addition of CuO species into CeO₂ promotes the reduction of Ce⁴⁺ and the creation of oxygen vacancy (V_O) defects. Raman analyses confirm V_O concentration initially increases and then decreases with the increasing CuO phase and the sample Ce1Cu2 exhibits the highest defect concentration. The room temperature ferromagnetic behavior is observed firstly in CeO₂/CuO nonmagnetic system and the maximal saturation magnetization appears in Ce1Cu2. The emergent ferromagnetism appears to be relevant to the extensive V_O defects, which can be interpreted by the indirect double-exchange model. The synthetic interaction between CeO₂ and CuO results in the redshift of the bandgap in prepared CeO₂/CuO nanocomposites.     

Thermal properties of Er:Li2TiGeO5 ferroelastic ceramics

Micron-grained (2–11 μm), erbium-doped, polycrystalline lithium titanium germinate ceramics were fabricated out of the heat-treated of the presintered samples at a temperature of 970 °C. X-ray diffraction showed a high crystallinity of the synthesized ceramics and confirmed formation of the natisite type structure with the P4/nmm symmetry. FE-SEM analysis revealed that the microstructure of obtained ceramics depends on dopant concentration. The number of pores increases with increasing the dopant dose. The specific heat measurements showed that the temperature of the ferroelastic phase transition was significantly reduced for Li₂TiGeO₅ ceramics (222 K) compared to the bulk (233.5 K). The investigations of the thermal conductivity showed its untypical behavior, proportional to the square of temperature, for a dielectric at low temperatures which could be explained by the microstructure of the samples.     

Effect of processing method on physical properties of Nb2O5

Samples of Nb₂O₅ were prepared by laser floating zone (LFZ) technique and by solid-state reaction in order to study some of their physical properties as a function of synthesis conditions. Single crystals fibres were obtained by LFZ, while a structural orthorhombic to monoclinic phase transition was observed in samples sintered at temperature higher than 800 °C. Transmission optical spectroscopy and photoconductivity measurements allowed identifying a ∼3.2 eV bandgap energy for the H-Nb₂O₅ monoclinic crystalline phase. Band gap shrinkage of ∼100 meV was observed from 14 K to RT. For the orthorhombic phase (T-Nb₂O₅), the photoconductivity measurements evidence a higher energy bandgap. The sintered samples have shown a broad recombination luminescence band at the orange/red spectral region while no luminescence was detected from the LFZ grown fibres. A dielectric constant of ∼40 was found for the 800 °C and 1200 °C sintered pellets while that of 1000 °C reached four times that value.