Microwave-assisted fast vapor-phase transport synthesis of MnAPO-5 molecular sieves

MnAPO-5 was prepared by a microwave-assisted vapor-phase transport method at 180 °C in short times. The products were characterized by X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectra, UV-vis spectroscopic measurement, NH₃-temperature-programmed desorption and esterification reaction. It was found that dry gels prepared with aluminum isopropoxide, phosphoric acid and manganese acetate could be transferred to MnAPO-5 in the vapors of triethylamine and water by the microwave-assisted vapor-phase transport method at 180 °C for less than 30 min. The crystallization time was greatly reduced by the microwave heating compared with the conventional heating. The resulting MnAPO-5 exhibited much smaller particle sizes, higher surface areas and slightly higher catalytic activity in the esterification of acetic acid and butyl alcohol than those prepared by the conventional vapor-phase transport method and hydrothermal synthesis.     

A low-temperature process to synthesize rutile phase TiO2 and mixed phase TiO2 composites

This works employed K₂Ti₄O₉, a novel Ti source, to prepare TiO₂ powders. By a “low-temperature dissolution-reprecipitation process” (LTDRP), rutile phase TiO₂ was successfully synthesized after reacting at 50 °C for 48 h. The obtained sample showed a specific surface area about 45 m²/g, and excellent activity in photo-destruction of NO_x gas. The coupling of rutile phase TiO₂ with commercial anatase TiO₂ showed significant effect in further enhancing the photocatalytic activity.     

Catalytic activity and magnetic properties of barium hexaferrite prepared from barite ore

Barium hexaferrite (BaFe₁₂O₁₉) has traditionally been used in permanent magnets and more recently used for high density magnetic recording. The classical ceramic method for the preparation of barium hexaferrite consists of firing mixture of chemical grade iron oxide and barium carbonate at high temperature. In this paper a mixture of chemical grade hematite, barium oxide and predetermined mixtures of iron oxide ore and barite ore containing variable amounts of coke were used to prepare barium hexaferrite (BaFe₁₂O₁₉) as a permanent magnetic material. The mixtures were mixed in a ball mill and fired for 20 h in a tube furnace at different temperatures (1100, 1150, 1200 and 1250 °C). XRD, magnetic properties, porosity measurements and catalytic activity were used for characterization of the produced ferrite. The results of experiments showed that the optimum conditions for the preparation of barium hexaferrite are found at 1200 °C for the mixture of chemical grade hematite and barium oxide. It was also found that the barium hexaferrite can be prepared from the iron and barite ores at 1200 °C. The addition of coke enhanced the yield of barium hexaferrite and improved its physicochemical properties. Samples prepared from ores with coke% = 0 show the most acidic active sites, they show a higher catalytic activity towards H₂O₂ decomposition. With addition of coke the catalytic activity decreases due to the poisoning effect of carbon on the available active site.     

Deposition-precipitation with Urea to prepare Au/Mg(OH)2 catalysts: Influence of the preparation conditions on metal size and load

Deposition-precipitation with Urea method to prepare Au/Mg(OH)₂ was investigated. The preparation was carried out at 80 °C using an aqueous solution of HAuCl₄ and Urea in presence of MgO as support precursor. The pH of the solution was 9.5-10 owing to the rapid hydration of MgO to Mg(OH)₂. The influence of the preparation conditions (Urea concentration, preparation procedure, addition of magnesium citrate) on the gold load and particle size distribution was evaluated. The structural characterization of preparations was carried out by means of X-ray diffractometry and transmission electron microscopy. Among the parameters investigated, the preparation procedure, that is the control of the interaction between gold species and the support, is the main step for the deposition of the highest amount of gold (> 80% of the theoretical amount) having small size and a narrow distribution (d = 4.1 nm, σ = ±1.1 nm). The synthesized catalysts were tested in the CO oxidation reaction.     

Vacuum ultraviolet optical properties of (La,Gd)PO4:RE (RE=Eu, Tb)

Vacuum ultraviolet excitation spectra of phosphors (La,Gd)PO₄:RE³⁺ (RE=Eu or Tb) and X-ray photoelectron spectra of LaPO₄ and GdPO₄ are investigated. The vacuum ultraviolet excitation intensity of (La,Gd)PO₄:RE³⁺ is enhanced with the increasing of Gd³⁺ content, which implies that Gd³⁺ plays an intermediate role in energy transfer from host absorption band to RE³⁺. When Gd³⁺ is doped into LaPO₄:Eu³⁺, charge transfer band (CT band) begins to shift to higher energy region and the overlap degree of CT band and the host absorption band gets greater with more Gd³⁺ doped into LaPO₄. These results suggest that the dopant (Gd³⁺) gives an important influence on energy transfer efficiency. The top of LaPO₄ valance band is formed by the 2p level of O²⁻, whereas that of GdPO₄ valance band is formed by the 2p level of O²⁻ and the 4f level of Gd³⁺, showing the differences in band structures between LaPO₄ and GdPO₄.     

Size-controlled synthesis of ZrO2-TiO2 nanoparticles prepared via reverse micelle method: Investigation of particle size effect on the catalytic performance in vapor phase Beckmann rearrangement

Zirconium-titanium mixed oxide nanoparticles have been synthesized using microreactors made of bis-(2-ethylhexyl) sulfosuccinate (AOT)/water/n-hexane microemulsions. The control of particle size was achieved by varying the process variables, such as water-to-surfactant molar ratio and reagent concentration. Their sizes, appearances, crystal structures, pore diameter and surface area were characterized by TEM, XRD, N₂ adsorption/desorption methods. The results revealed that samples prepared in reverse micelles had no crystalline phase. The Beckmann rearrangement of cyclohexanone oxime on ZrO₂-TiO₂ nanoparticles was carried out in a fixed-bed down flow reactor to investigate the effect of particle size on catalytic activity and selectivity. Samples synthesized in reverse micelles had better reaction performance than samples prepared via sol-gel method. A parallel relationship could be drawn between the catalytic activity and the particle size as well as the selectivity of the catalyst.     

The synthesis of monoclinic bismuth vanadate nanoribbons and studies of photoconductive, photoresponse, and photocatalytic properties

Large-scale, high-purity and uniform BiVO₄ nanoribbons have been synthesized by a facile hydrothermal route without surfactants. The as-prepared BiVO₄ nanoribbons were up to hundreds of micrometers in length, 60-80 nm in width, 15-20 nm in thickness, and grew along the [0 1 0] direction. The photoresponse property of BiVO₄ nanoribbons was measured under different wavelengths. Their photoswitch behavior was also demonstrated. Furthermore, the nanoribbons showed superior photocatalytic activities in the degradation of eosin Y under visible light irradiation.     

Effects of pH on morphosynthesis and photocatalytic activity of calcium titanium oxides via a facile aqueous strategy

By controlling pH values, calcium titanium oxides with various morphologies had been synthesized via a simple hydrothermal route. No surfactants or templates were involved in the shaping process. The results found that pH values had a crucial effect on the crystal phase and shape evolution of the samples. With increasing pH values, the obtained sample changed from one-dimension (1D) CaTi₂O₅ rod or shuttle-like shape to two-dimension (2D) CaTi₂O₄(OH)₂ nanosheets, and then to three-dimension (3D) CaTiO₃ aggregated prisms, butterfly-like dendrites and cross cubic shapes. The formation mechanism was proposed for the evolution of phase and morphology. 3D CaTiO₃ butterfly-like sample showed good photocatalytic activity due to unique morphology, enhanced light harvesting and large surface area.     

Preparation of nitrogen doped TiO2 photocatalyst by oxidation of titanium nitride with H2O2

Nitrogen doped anatase TiO₂ (N-TiO₂) were prepared by hydrothermally treating TiN with H₂O₂. The as-synthesized samples were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), UV-vis diffuse reflectance spectrum (DRS), Fourier transform infrared spectra (FT-IR) and X-ray photoelectron spectroscopy (XPS) techniques. The results confirmed that the hydrothermal oxidation is an effective method to prepare N-doped TiO₂ anatase. The nitrogen concentration in TiO₂ could be controlled by the concentration of H₂O₂ solution. Photocatalytic degradation of methyl orange (MO) was carried out under visible light and UV-visible light irradiation, respectively. The as-prepared optimal N-TiO₂ showed higher photocatalytic activity than N-P25 and P25, and exhibited excellent reusability.     

Sub-2 nm SnO2 nanocrystals: A reduction/oxidation chemical reaction synthesis and optical properties

A simple reduction/oxidation chemical solution approach at room temperature has been developed to synthesize ultrafine SnO₂ nanocrystals, in which NaBH₄ is used as a reducing agent instead of mineralizers such as sodium hydroxide, ammonia, and alcohol. The morphology, structure, and optical property of the ultrafine SnO₂ nanocrystals have been characterized by high-resolution transmission electron microscopy (HRTEM), X-ray powder diffraction (XRD), differential scanning calorimetry and thermogravimetric analysis (DSC-TGA), X-ray photoelectron spectroscopy (XPS) and UV-vis absorption spectroscopy. It is indicated that the uniform tetragonal ultrafine SnO₂ nanocrystals with the size below 2 nm have been fabricated at room temperature. The band gap of the ultrafine SnO₂ nanocrystals is about 4.1 eV, exhibiting 0.5 eV blue shift from that of the bulk SnO₂ (3.6 eV). Furthermore, the mechanism for the reduction/oxidation chemical reaction synthesis of the ultrafine SnO₂ nanocrystals has been preliminary presented.     

Solid-phase reaction synthesis of mesostructured tungsten disulfide material with a high specific surface area

A mesostructured tungsten disulfide (WS₂) material was prepared through a solid-phase reaction utilizing ammonium tetrathiotungstate as the precursor and n-octadecylamine as the template. The as-synthesized WS₂ material was characterized by X-ray powder Diffraction (XRD), Low-temperature N₂ Adsorption (BET method), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM). The characterization results indicate that the WS₂ material has the typical mesopore structure (3.7 nm) with a high specific surface area (145.9 m²/g), and large pore volume (0.18 cm³/g). This approach is novel, green and convenient. The plausible mechanism for the formation of the mesostructured WS₂ material is discussed herein.     

IF-WS2 nanoparticles size design and synthesis via chemical reduction

An innovative synthesis of inorganic fullerene-like disulfide tungsten (IF-WS₂) nanoparticles was developed using a chemical reduction reaction in a horizontal quartz reactor. In this process, first tungsten trisulfide (WS₃) was formed via a chemical reaction of tetra thiotungstate ammonium ((NH₄)₂WS₄), polyethylene glycol (PEG), and hydrochloric acid (HCl) at ambient temperature and pressure. Subsequently, WS₃ was reacted with hydrogen (H₂) at high temperature (1173-1373 K) in a quartz tube. The produced WS₂ nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDAX), and transmission electron microscopy (TEM). The characterization results indicated that the high-purity (100%) IF-WS₂ nanoparticles were produced. Moreover, addition of surfactant (PEG) and higher operating temperature (1173-1373 K) decreased the particles agglomeration, and consequently led to the reduction of average diameter of WS₂ particles in the range of 50-78 nm. The developed method is simple, environmentally compatible, and cost-effective in contrast to the conventional techniques.     

Facile 1,4-dioxane-assisted solvothermal synthesis,optical and electrochemical properties of CeO2 microspheres

CeO₂ microspheres, with an average diameter of 1 μm, have been successfully prepared through a facile 1,4-dioxane-assisted solvothermal synthesis, where 1,4-dioxane is acted as a capping agent for the first time. By varying the solvent ratio, the formation mechanism for the CeO₂ microspheres has been proposed on an isotropic growth through the capping function of 1,4-dioxane. The strong UV–vis spectra result indicates that the CeO₂ microspheres are suitable as an UV blocking and shielding material. The cyclic voltammetric measurements of hemoglobin immobilized on CeO₂-Nafion modified glassy carbon electrode reveal a typical characteristic of surface-controlled thin-layer electrochemical behavior of the CeO₂ microspheres.     

Novel hydrothermal synthesis method for tobermorite fibers and investigation on their thermal stability

Tobermorite fibers have been successfully synthesized by hydrothermal reaction at 200°C under the pressure of 2 MPa after 3-10 h using a Ca(II)-EDTA complex precursor. XRD patterns, TG-DTA analysis, and SEM observations show that the products are needle-like tobermorite fibers, which have diameter, length, and aspect ratio in the range of 0.1-10, 40-100, and 20-80 μm, respectively. The fibers can maintain their shapes up to 1150°C during the heat treatment.     

The microwave effect on the properties of silica-coated TiO2 fine particles prepared using sol-gel method

The silica coating of TiO₂ fine particle was conducted using microwave assisted sol-gel method and conventional sol-gel method to suppress its photo-catalytic activity. The amount and uniformity of silica coating on TiO₂ surface were characterized by X-ray photoelectron spectroscopy (XPS), X-ray fluorescence spectroscopy (XRF), infrared spectroscopy (IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and zeta potential measurements. XPS and XRF results showed that the presence of catalyst and reaction time were important factors to reach high silica amounts. SEM, TEM, and zeta potential results indicated that dense film coating of SiO₂ layer formed on TiO₂ surface in conventional sol-gel method, whereas the nucleation coating was observed on sample prepared by microwave assisted sol-gel method. When photo-catalytic activities and ultraviolet (UV) shielding abilities of these samples were evaluated, the sample prepared by microwave processing showed higher inhibition of photo-catalytic activity and better UV shielding ability than the sample prepared by conventional method. These results suggested that the coating method significantly affected the photo-catalytic activity and UV shielding ability of coated TiO₂.     

Strontium vanadate nanoribbons: Synthesis, characterization and detection of dopamine

Large-scale, high-purity and uniform strontium vanadate (Sr₂V₂O₇) nanoribbons were easily synthesized via a hydrothermal process without any surfactants. The as-prepared products were up to hundreds of micrometers in length, 200-600 nm in width, and 20 nm in thickness. These nanomaterials were employed to modify glassy carbon electrode, which displayed excellent electrochemical sensitivity in detecting dopamine in the presence of ascorbic acid. A linear relationship between the concentrations of dopamine and its oxidation peak currents was obtained. The modified electrode exhibited high reproducibility and stability, which might be found potential application in the biosensors.     

Surfactant-free synthesis and electrochemical properties of chrysanthemum-like InVO4 hierarchical microstructures

Novel chrysanthemum-like hierarchical microstructures of orthorhombic InVO₄ were synthesized via a hydrothermal route without assistance of any template or organic additive. The chrysanthemum-like InVO₄ microstructures are built up of numerous nanobelts radially aligned around the spherical surface. Based on the structural feature of orthorhombic InVO₄ and the key role of the pH value, a probable mechanism of the etching-splitting growth process induced by H⁺ ions was proposed to explain the formation of InVO₄ microstructures. Furthermore, the chrysanthemum-like InVO₄ sample shows a high discharge capacity of 608.6 mAh g⁻¹ and acceptable capacity retention when used as an electrode material in lithium ion batteries. The pure orthorhombic phase and unique porous morphology play basic roles in the structural requirement to serve as transport paths for lithium ion.     

Synthesis of flower- and rod-like nickel sulfide nanostructures by an organic-free hydrothermal process

Well-crystalline flower- and rod-like NiS nanostructures have been synthesized by an organic-free hydrothermal process at a low temperature of 200 °C. X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) were employed to characterize the as-synthesized NiS nanostructures. The effects of temperature and reaction time on the morphology have been also investigated. The two-step flake-cracking mechanism for the formation of flower- and rod-like NiS nanostructures was discussed. The products were also investigated by photoluminescence (PL) spectroscopy.     

Sintering and dielectric properties of BaTiO3 prepared by a composite-hydroxide-mediated approach

High purity tetragonal BaTiO₃ powders consisted of uniform particles of ca. 150 nm in diameter were synthesized by a composite-hydroxide-mediated approach at 240 °C using a novel hydrothermal reaction apparatus with a rolling system. The product showed sinterability superior to the commercial powder, i.e., it could be sintered to full theoretical density at 1200 and 1100 °C without an additive and with 0.3 wt% of Li₂CO₃-0.04 wt% of V₂O₅ mixed sintering aid, respectively. The sintered body of the product also showed piezoelectric properties superior to the commercial one.     

Effect of pH value on particle morphology and electrochemical properties of LiFePO4 by hydrothermal method

Lithium iron phosphate was prepared by hydrothermal synthesis using LiOH·H₂O, FeSO₄·7H₂O and H₃PO₄ as raw materials. The effects of pH value of reaction solution on particle morphology and electrochemical property were investigated. The pH value of the reaction solution was adjusted in the range of 2.5-8.8 by dilute sulfuric acid and ammonia water. The samples were characterized by field-emission scanning electronic microscope (FE-SEM), X-ray powder diffraction (XRD), constant-current charge/discharge cycling tests and chemical analysis. The results indicated that the particles exhibited acute angle diamond flake-like morphology at pH = 2.5, and as the pH value increased, the particle became hexagon flake-like, round flake-like and irregular flake-like morphology gradually. The optimal sample synthesized at pH = 6.4 exhibited discharge capacities of 151.8 mAh g⁻¹ at 0.2 C rate and 129.3 mAh g⁻¹ at 3 C rate. It was found that pH value affected the morphologies and properties of the product by means of different crystal growth rates.