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.     

Investigation of the conditions for synthesis of Ce<Subscript>0.9</Subscript>Y<Subscript>0.1</Subscript>O<Subscript>2</Subscript> dense coatings

The conditions for preparation of Ce_0.9Y_0.1O₂ (CYO) oxide coatings on La_0.8Sr_0.2MnO₃ (LSM) ceramic substrates by screen printing were investigated. The CYO compound was synthesized by the pyrolysis of polymer-salt composites with the aim of producing submicron powders with a uniform size distribution. Transmission electron microscopy of the microstructure of the CYO compound synthesized with ethylene glycol revealed that the synthesis product consists of ultrafine crystalline particles with an average size of 5–15 nm. The use of CYO nanopowders made it possible to prepare rather dense single-layer coatings on LSM substrates. It was demonstrated that annealing of the coatings at high temperatures leads to the recrystallization and coarsening of particles.     

Effect of preparation temperature on the formation of Sr2CeO4 phosphor particles in the spray pyrolysis

Sr₂CeO₄ phosphor particles were prepared by spray pyrolysis at various preparation temperatures. The effect of preparation temperatures on the morphology, crystal structure and photoluminescence characteristics of the post-treated Sr₂CeO₄ phosphor particles was studied. Phase pure Sr₂CeO₄ phosphor particles were not produced by spray pyrolysis without post-treatment. The optimum post-treatment temperature to produce the Sr₂CeO₄ phosphor particles with high photoluminescence intensity was 1,000 °C in spray pyrolysis. The spherical morphology of the as-prepared particles obtained at high preparation temperatures above 1,400 °C had maintained after post-treatment at 1,000 ‡C. The relative photoluminescence intensities of the Sr₂CeO₄ phosphor particles varied with the preparation temperatures in the spray pyrolysis. The as-prepared particles obtained by spray pyrolysis at preparation temperatures below 1,400 °C converted into phase pure Sr₂CeO₄ phosphor particles after post-treatment at 1,000 ‡C. The optimum preparation temperature of the as-prepared particles was 1,400 °C to produce the Sr₂CeO₄ phosphor particles with spherical shape and high photoluminescence intensity in the spray pyrolysis.     

Spray pyrolysis synthesis of mesoporous TiO<Subscript>2</Subscript> microspheres and their post modification for improved photocatalytic activity

Mesoporous TiO₂ microspheres were prepared by spray pyrolysis for photocatalysis. Post modification of TiO₂ by heat treatment was performed to optimize its photocatalytic performance. First, spherical TiO₂ particles with mesoporous structure were synthesized at pyrolysis temperatures of 500, 600, and 700 °C. After characterization by XRD, SEM, and N₂ adsorption, a sample prepared at 500 °C was found to possess desirable properties for photocatalytic performance through post-modification. In methylene blue degradation, mesoporous TiO₂ microspheres synthesized at 500 °C outperformed other microspheres. Furthermore, samples obtained by spray pyrolysis at 500 °C were calcined at various temperatures as a post-modification process. The sample calcined at 350 °C showed improved photocatalytic activity due to optimal anatase crystallinity and surface area.     

Controllable crystallite and particle sizes of WO3 particles prepared by a spray‐pyrolysis method and their photocatalytic activity

Information about correlation of material properties parameters (i.e., crystallite and particle sizes) and photocatalytic activity of tungsten trioxide (WO₃) particles are still lacking. For this reason, the purpose of this study was to synthesize WO₃ particles with controllable crystallite (from 18 to 50 nm) and particle sizes (from 58 to 677 nm) using a spray‐pyrolysis method and to investigate correlation of crystallite/particle size and photocatalytic activity. To gain control of crystallite/particle size, synthesis temperature (120–1300^°C) and initial precursor concentration (2.5–15 mmol/L) were investigated, which were then compared with the proposal of the particle formation mechanism. The results showed that both crystallite and particle sizes played an important role in photocatalytic activity. In this research, the optimum condition to produce the highest photocatalytic performance of WO₃ particles was at the temperature of 1200^°C (crystallite size: 25 nm), and initial concentration of 10 mmol/L (particle size: 105 nm). © 2013 American Institute of Chemical Engineers AIChE J, 60: 41–49, 2014     

Effects of adding B<Subscript>2</Subscript>O<Subscript>3</Subscript> as a flux on phosphorescent properties in synthesis of SrAl<Subscript>2</Subscript>O<Subscript>4</Subscript>: (Eu<Superscript>2+</Superscript>, DY<Superscript>3+</Superscript> phosphor

SrAl₂O₄: (Eu²⁺, Dy³⁺) phosphor was prepared by solid state reaction. B₂O₅ as a flux was added in SrAl₂O₄:(Eu ²⁺, Dy³⁺) in order to accelerate a solid state reaction. In this paper, the effects of B₂O₃ on the crystal structure and the phosphorescent properties of the material have been evaluated. The synthesized phosphor exhibited a broad band emission spectrum peaking at 520 nm, and the spectrum peak showed little effect by the B₂O₃ contents. The maximum afterglow intensity of the SrAl₂O₄: (Eu²⁺, Dy³⁺) phosphor was obtained at the B₂O₃ content of 5%. Adding the B₂O₃ caused uniform distortion to the crystal structure of the phosphor and resulted in reducing the lengths of a and c axes and Β angle of the SrAl₂O₄ crystal. The uniform distortion was accompanied with crystal defects which can trap the holes generated by the excitation of Eu²⁺ ions. The afterglow characteristic of the SrAl₂O₄: (Eu²⁺, Dy³⁺) phosphor was thus enhanced.     

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.     

Synthesis of nanometer sized Bi<Subscript>2</Subscript>WO<Subscript>6</Subscript>s by a hydrothermal method and their conductivities

Nanometer-sized bismuth tungsten oxides, Bi₂WO₆s, were successfully synthesized by hydrothermal treatment at 200 °C for 24 hr, and their morphologies and crystallite sizes were influenced by adjusting the conditions to pH 4, 7, and 9. TEM images revealed that the particles were sheet-shaped and the crystallite sizes ranged from 7–120 nm. The samples absorbed in the visible range at about 380–400 nm. The lowest conductivity, 1.0×10⁶ ohm/square, was observed for Bi₂WO₆ prepared at pH 4 with a 150 nm film thickness. As the annealing temperature for Bi₂WO₆ prepared at pH 7 was increased, the conductivity decreased due of formation of larger particles by coagulation and sintering at high temperatures. Conductivity appears to improve with increasing film thickness up to 1,500 nm.     

Morphologies and properties of NiO particles prepared from NiCl<Subscript>2</Subscript>·6H<Subscript>2</Subscript>O by spray pyrolysis

Nickel oxide particles were prepared by spray pyrolysis of aqueous solution of NiCl₂·6H₂O. In the reactor the salt droplets were first converted to hollow particles by drying and then they were collapsed by oxidation to reduce their size. Each oxide particle was composed of many small nuclei with voids among them due to extremely low rate of sintering. The particle size decreased with the temperature as the sintering and crystallization proceeded. The size as well as the crystallinity of the particles increased with the initial salt concentration. When the salt droplets were preliminarily dried in diffusion dryer before entering the reactor, the collapse of the particles was considerably reduced, resulting in lower hollowness and higher sphericity. Numerical simulation on the drying of the droplets provided insight on the initial stage of spray pyrolysis.     

Synthesis and sintering of Gd-doped CeO2 nanopowders prepared by ultrasonic spray pyrolysis

Ultrasonic spray pyrolysis (USP) of nitrate-based precursors was used to fabricate fine and polycrystalline Ce_0.8Gd_0.2O_1.9 (CGO) powders with controlled microstructure in a one-step process varying four spray-pyrolysis parameters: precursor solution concentration, atomizing frequency, carrier gas flow rate, and pyrolysis temperature. A design of experiment (DOE) was used to understand the independent and combined influences of these process parameters on the particle size, particle size distribution and crystallite size. In this study, smaller CGO particles with narrower particle size distribution and finer grain size showed a full densification starting at a low temperature. CGO densification was found to be strongly dependent on CGO powder microstructural properties.     

Particle deposition behaviors of monolithic De-NO<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> catalysts for selective catalytic reduction (SCR)

A major issue when using selective catalytic reduction (SCR) De-NO _x catalysts is the risk of physical deactivation due to particle deposition and plugging of the monolithic catalysts. In the present study, numerical computations were carried out to investigate the particle deposition behaviors in monolithic SCR catalysts. Based on the calculation results, the effects of particle diameter, particle density, gas velocity, turbulent intensity, chemical reaction and channel size on particle deposition were analyzed in detail. Increasing gas velocity and equivalent diameter of channel can mitigate particle deposition. The increases of turbulent intensity and channel length both lead to the rise of particle deposition ratio. For particles with high Stokes number, particle deposition mainly takes place in the inlet section of catalysts. For particles with low Stokes number, sediment can be observed in the middle and outlet sections of catalysts. De-NO _x chemical reaction can mitigate particle deposition, but the effect of chemical reaction on particle deposition is inactive.     

Combustion of metallothermic mixtures FeO-Cr<Subscript>2</Subscript>O<Subscript>3</Subscript>-Al-C: Influence of carbon granularity and localization

Combustion of metallothermic mixtures FeO-Cr₂O₃-Al-C in air at normal conditions was studied upon variation in the size of carbon (graphite) particles and carbon localization in a green sample. Carburization conditions were optimized in terms of graphite particle size.     

Effect of synthesis condition and annealing on the sensitivity and stability of gas sensors made of Zn-doped <Emphasis Type="Italic">γ</Emphasis>-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> particles

Gas sensors made of flame-synthesized Zn-doped γ-Fe₂O₃ nanoparticles were found to have high sensitivity and high aging resistance. Zinc-doped γ-Fe₂O₃ nanoparticles and microparticles were synthesized by flame spray pyrolysis (FSP). Gas sensors were fabricated with as-synthesized particles, and with particles that had been annealed. The sensors’ response to acetone vapor and H₂ was measured as fabricated, and measured again after the sensors were aged for three days. The sensors made from as-synthesized particles showed a gas sensing sensitivity 20 times higher than the literature value. However, sensors made of microparticles lost their sensing ability after three days of aging; sensors made of nanoparticles retained their gas sensing capability after aging. Sensors made of annealed particles did not have significant gas sensing capabilities. Analysis using the William and Hall method showed that the microstrains decreased significantly in both H₂/O₂ and H₂/Air flame synthesized particles after annealing. The results showed that sensors made of flame-synthesized particles have much higher sensitivity than sensors made of particles previously reported. Especially, sensors made of flame-synthesized nanoparticles are resistant towards aging. This aging resistance may be attributed to the particles’ ability to retain their microstrains.     

Microwave-assisted dissolution of UO<Subscript>2</Subscript> with TBP-HNO<Subscript>3</Subscript> complex

The direct dissolution of UO₂ in TBP-HNO₃ complex by microwave heating in this study suggests the possibility of dissolving spent nuclear fuels. This new technique offers many benefits for reduction in aqueous and organic waste generation and improved efficiency of chemical processing. The dissolution rate of UO₂ particles with TBP-HNO₃ complex by microwave assisted heating is highly dependent on the temperature and the particle size.     

Preparation of TiO<Subscript>2</Subscript>/SiO<Subscript>2</Subscript> hollow spheres and their activity in methylene blue photodecomposition

PSA [poly-(styrene-methyl acrylic acid)] latex particle has been taken into account as template material in SiO₂ hollow spheres preparation. TiO₂-doped SiO₂ hollow spheres were obtained by using the appropriate amount of Ti(SO₄)₂ solution on SiO₂ hollow spheres. The photodecomposition of the MB (methylene blue) was evaluated on these TiO₂-doped SiO₂ hollow spheres under UV light irradiation. The catalyst samples were characterized by XRD, UV-DRS, SEM and BET. A TiO₂-doped SiO₂ hollow sphere has shown higher surface area in comparison with pure TiO₂ hollow spheres. The 40 wt% TiO₂-doped SiO₂ hollow sphere has been found as the most active catalyst compared with the others in the process of photodecomposition of MB (methylene blue). The BET surface area of this sample was found to be 377.6 m²g⁻¹. The photodegradation rate of MB using the TiO₂-doped SiO₂ catalyst was much higher than that of pure TiO₂ hollow spheres.     

Green-emitting yttrium silicate phosphor particles prepared by large scale ultrasonic spray pyrolysis

Tb doped Y₂SiO₅ phosphor particles with spherical morphology, fine size, high crystallinity and good photoluminescence intensity were prepared by spray pyrolysis. The colloidal solution obtained by adding the fumed silica particles was introduced to control the characteristics of Y₂SiO₅: Tb phosphor particles. The particles prepared from the colloidal solution had a spherical and filled morphology even after post-treatment. The particles post-treated below 1,200 ‡C had X1 type crystal structure but the crystal structure changed from X1 to X2 after post-treatment above 1,300 ‡C. When crystal structure was changed from X1 to X2, the PL intensity greatly increased. The maximum PL intensity of particles, which were prepared from the solution with 120% excess of stoichiometric fumed silica, was about 4 times higher than that of the particles prepared from the stoichiometric solution. The particles prepared from the stoichiometric solution of yttrium nitrate and fumed silica had mixed phases of X1 and X2 type and had impurity as Y₂O₃. On the other hand, the particles prepared from the solution with 120% excess of stoichiometric fumed silica had high crystallinity of X2 type.     

Kinetics and mechanism of the formation of hollandites in the BaO(Cs<Subscript>2</Subscript>O)-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiO<Subscript>2</Subscript> system from initial mixtures prepared by different methods

The mechanism and kinetics of formation of solid solutions based on hollandite in the BaO(Cs₂O)-Al₂O₃-TiO₂ system are investigated using the initial mixtures prepared by two methods: (i) mechanical grinding and mixing of the initial components and (ii) coprecipitation from aqueous solutions of the salts. It is established that the mechanism of formation of hollandite in the system under investigation depends on the degree of dispersion of the initial mixtures used in the synthesis. When the synthesis is performed with the initial mixture prepared by mechanical grinding and mixing of the initial reactants (the particle size is equal to 50–300 nm), hollandite is formed at temperatures in the range 1100–1250°C in the presence of the accompanying phase Cs₂Al₂Ti₂O₈. When the synthesis is performed with the initial mixture prepared by coprecipitation from aqueous solutions of salts (the particle size is equal to 10–12 nm), hollandite is formed at temperatures in the range 850–1050°C. The investigation into the kinetics of formation of the hollandite phase from the above mixtures made it possible to determine the temperature-time conditions for the synthesis of this titanate in the form of a powder with a particle size of approximately 50 nm or in the form of a dense ceramic material with a particle size of ～200 nm.     

Effect of surface modification of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles on the preparation of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/polystyrene composite particles via miniemulsion polymerization

Fe₃O₄ nanoparticles were modified by n-octadecyltrimethoxysilane (C18TMS) and 3-trimethoxysilylpropylmethacrylate (MPS). The modified Fe₃O₄ nanoparticles were used to prepare Fe₃O₄/polystyrene composite particles by miniemulsion polymerization. The effect of surface modification of Fe₃O₄ on the preparation of Fe₃O₄/polystyrene composite particles was investigated by transmission electron microscopy, Fourier transform infrared spectrophotometer (FT-IR), contact angle, and vibrating sample magnetometer (VSM). It was found that C18TMS modified Fe₃O₄ nanoparticles with high hydrophobic property lead to the negative effect on the preparation of the Fe₃O₄/polystyrene composite particles. The obtained composite particles exhibited asymmetric phase-separated structure and wide size distribution. Furthermore, un-encapsulated Fe₃O₄ were found in composite particles solution. MPS modified Fe₃O₄ nanoparticles showed poor hydrophobic properties and resulted in the obtained Fe₃O₄/polystyrene composite particles with regular morphology and narrow size distribution because the ended C=C of MPS on the surface of Fe₃O₄ nanoparticles could copolymerize with styrene which weakened the phase separation distinctly.     

Soft Template Synthesis of Super Paramagnetic Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> Nanoparticles a Novel Technique

The present study reports a facile technique for the synthesis of crystalline super paramagnetic nano ferrite (Fe₃O₄) particles using diethyl amine as a soft template. The spectral properties of Fe₃O₄ nanoparticles were characterized by UV–visible and Fourier Transform Infrared (FTIR) spectroscopies while the crystalline structure and particle size was estimated using X-Ray diffraction (XRD) as well as transmission electron microscopy (TEM) techniques. The super paramagnetic behavior of Fe₃O₄ nanoparticles was determined using vibrating sample magnetometer (VSM) at 300 K. The results of the studies revealed that this technique could be adopted to synthesize agglomerate free super paramagnetic Fe₃O₄ nanoparticles which may find potential application in the filed of biosensor and corrosion protective coatings.     

Sodium Carbonate Flux Effects on the Luminescence Characteristics of (Y0.5Gd0.5)2O3:Eu Phosphor Particles Prepared by Spray Pyrolysis

Na₂CO₃ flux was introduced in the preparation of phosphor particles by spray pyrolysis to improve the photoluminescence (PL) characteristics of (Y_0.5Gd_0.5)₂O₃:Eu phosphor particles. The phosphor particles directly prepared by spray pyrolysis at 1300°C from solutions with 20 wt% Na₂CO₃ flux had the highest PL intensity, which corresponded to 130% of that of particles prepared from solution without flux. On the other hand, the maximum PL intensity of the annealed particles, which were as-prepared at 900°C and posttreated at 1200°C for 3 h, was obtained from a solution with 5 wt% Na₂CO₃ flux. The maximum PL intensity of particles directly prepared by spray pyrolysis without posttreatment was 86% of that of posttreated phosphor particles. Na₂CO₃ flux was also important in control of morphology of (Y_0.5Gd_0.5)₂O₃:Eu phosphor particles.