Ultrasonic-assisted synthesis of Ce doped cubic–hexagonal ZnTiO3 with highly efficient sonocatalytic activity

Ce doped ZnTiO₃ as a novel catalyst with highly efficient and stable sonocatalytic activity was synthesized via an ultrasound-assisted sol–gel method using non-ionic surfactant Pluronic F127 as structure directing agent. Synthesized samples were characterized by using various techniques, such as XRD, TEM, SEM, EDX, ​XRF, BET, DRS, and PL, and their sonocatalytic activity studied toward degradation of p-Nitrophenol as a model organic compound. The synthesized mesoporous Ce/ZnTiO₃ had mixed cubic–hexagonal phase with large surface area (118.2 m² g^–1) and narrow pore size distribution (4.9 nm). The effects of cerium concentration, calcination temperature, and calcination time on the structure and the sonocatalytic activity of Ce/ZnTiO₃ were studied in detail. XRD results were suggested that the relation between the phase structure and the catalytic activity is considerable. Significant decrease in band-gap and PL intensity was observed with increasing the cerium concentration in the ZnTiO₃. It became clear that the Ce/ZnTiO₃ (0.81 mol%) shows high sonocatalytic activity compared with pure ZnTiO₃ and other Ce/ZnTiO₃ samples as well as commercial TiO₂-P25. The possible mechanism for the enhanced sonocatalytic activity of Ce/ZnTiO₃ was discussed in details. The electrical energy consumption was also considered during sonocatalytic experiments.     

Formal Mott transition between the one dimensional conductor K0.3MoO3 and the highly anisotropic semiconductor K0.33MoO3

The blue bronze K_0.3MoO₃ (1) is well known to have a 1-D character along the crystallographic b axis. The red bronze K_0.33MoO₃, instead, is a semiconductor with a 0.5 eV energy gap (2). The two bronzes have a different crystallographic configuration. In a microscopic model one can derive the red bronze structure from the one of the blue bronze and one can explain the metal semiconductor “transition” between K_0.3MoO₃ and K_0.33MoO₃ with a formal Mott transition of delocalized into localized states due to a critical overlap between cationanion-cation orbitals.     

Ultrasonic-assisted size-controllable synthesis of Bi2Te3 nanoflakes with electrogenerated chemiluminescence

Bi(2)Te(3) hexagonal nanoflakes with controllable edge length ranging from approximately 150 nm to as small as approximately 10nm were synthesized via an ultrasonic-assisted disproportionation route, using Te powder and Bi(NO(3))(3).5H(2)O as raw materials. The mechanochemical effects of the ultrasonic irradiation accelerated the reaction and were helpful to obtain relatively small and uniform nanocrystals. The products were characterized by X-ray powder diffraction, X-ray photoelectron spectra, transmission electron microscopy, and selected area electron diffraction techniques. Electrogenerated chemiluminescence of as-prepared Bi(2)Te(3) was also reported for the first time.     

Controlled synthesis of cuprous oxide nanospheres and copper sulfide hollow nanospheres

Uniform Cu₂O nanospheres have been successfully synthesized by reducing CuSO₄ with ascorbic acid in sucrose solution at room temperature. The diameter of the Cu₂O nanospheres can be tuned from 90 to 280 nm by adding different amounts of sucrose in the solution. Furthermore, CuS hollow nanospheres with different diameters have been obtained based on the Kirkendall effect using the as-prepared Cu₂O nanospheres as sacrificial templates. Cu₂O/Cu_7.2S₄ core/shell nanospheres and Cu_7.2S₄ hollow nanospheres are obtained as the intermediate products at different stages of the conversion process. Through the post-treatment of sodium citrate solution, Cu_7.2S₄ hollow nanospheres can be changed into CuS hollow nanospheres. The products are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and field-emission scanning electron microscopy (FESEM). Optical properties of the products have also been studied.     

Structural study of highly dispersed cerium dioxides

Cerium dioxide samples of different dispersivity, obtained by different methods, have been investigated by X-ray diffraction (XRD) analysis, full-profile analysis of diffraction patterns, calculation of radial distribution function (RDF) of electron density, and extended X-ray absorption fine-structure (EXAFS) spectroscopy. According to the XRD data, the samples studied can be identified in the fluorite structure with conventional unit-cell parameters. However, the local structure of highly dispersed samples, determined by the RDF and EXAFS methods, changes: the coordination spheres for the Ce-O distances are represented by two distances.     

Ultrasonic-assisted synthesis of flavones by oxidative cyclization of 2′-hydroxychalcones using iodine monochloride

This paper presents an efficient methodology for the synthesis of flavones via the oxidative cyclization of 2′-hydroxychalcones in the presence of iodine monochloride with DMSO under ultrasound irradiation. Ultrasonic irradiation enhances the cyclization reaction and leads to reduced reaction time at lower reaction temperatures while generating flavones with high yields.     

Low-temperature synthesis of morphology controlled metastable hexagonal molybdenum trioxide (MoO3)

We demonstrate a simple low-temperature chemical method to produce metastable hexagonal MoO₃ phase nanorods. The structure, chemical purity, thermal stability and optical properties of hexagonal MoO₃ are reported. Our results provide a more direct method to produce high quality and stable hexagonal MoO₃, which exhibits phase stability up to 400 ^°C at which point an irreversible phase transition occurs to form orthorhombic MoO₃.     

Preparation of highly dispersed MgO and its bactericidal properties

Samples of layered double hydroxides (LDHs) were prepared by a method involving separate nucleation and aging steps recently developed in our laboratory, using varying [ Mg²⁺] /[ Al³⁺] ratios and different aging conditions. The samples were characterized by X-ray diffraction (XRD), FT-IR spectroscopy and laser granulometry. The results showed that LDHs with different particle sizes could be obtained by controlling the reaction temperature and degree of supersaturation. Calcination of these materials affords mixtures of highly dispersed MgO and mixed metal oxides. Bactericidal experiments against Bacillus subtilis var. niger and Staphylococcus aureus were carried out using materials formed by calcination of the LDHs at 500 ^○C. The mechanism of bactericidal activity was also investigated. It is known that MgO is very readily hydrated and that reaction with dissolved oxygen affords superoxide anions O₂^-, which attack the secondary amide structure of proteins leading to destruction of the bacteria. The bactericidal activity of the MgO increases with specific surface area because this leads to an increased number of surface hydroxyl groups and higher concentrations of O₂^- in solution. The bactericidal ability of MgO therefore increases with decreasing particle size.     

Polymer adsorption on the surface of highly dispersed silica

Attempts at modification of silica surface with a polymer (natural latex) directly in the course of the precipitation process have been made. The effects of temperature, non-ionic surfactants and silane coupling agent in preparation of poly[cis-isoprene]-coated silica on the precipitation of polymer/silica composites initiated by ammonium salts (NH₄Cl, (NH₄)₂SO₄, NH₄HCO₃), have been studied. The influence of the process parameters on the quality of the silicas obtained and the character of the polymer adsorption on the silica surface has been determined along with the effect of the surface impregnation with natural latex on physicochemical parameters of the silicas (bulk density, capacities to absorb water, dibutyl phthalate and paraffin oil) and their surface structure.     

Organized and highly dispersed growth of MnO2 nano-rods by sonochemical hydrolysis of Mn3acetate

Highly dispersed and non-agglomerated alpha-MnO(2) nano-needles of dimensions 20-30 nm have been synthesized by the application of ultrasound radiation on the aqueous solution consisting of manganese(3)acetate close to neutral pH followed by mild drying. With a similar reaction system, hot hydrolysis (non-sonochemical process) produced beta-MnO(2) nano-rods of length 100-200 nm but with high degree agglomeration. Sonochemical cavitation phenomenon is suggested to have a pronounced effect for the formation of special phase and morphology. The effect is proved by the difference in the intermediate products which has difference in crystalinity and phase-purity. The intermediate phases are identified to be single-phase gamma-MnOOH for the non-sonochemical reaction and mixture of gamma-MnOOH, alpha-MnO(2) and beta-MnO(2) for the sonochemical products.     

Ultrasonic-assisted ultra-rapid synthesis of monodisperse meso-SiO2@Fe3O4 microspheres with enhanced mesoporous structure

A core–shell-type of meso-SiO₂@Fe₃O₄ microsphere was synthesized via an ultrasonic-assisted surfactant-templating process using solvothermal synthesized Fe₃O₄ as core, tetraethoxysilane (TEOS) as silica source, and cetyltrimethyl ammonium bromide (CTAB) as templates. The samples were characterized by FT-IR, XRD, TEM, N₂ adsorption–desorption technology, and vibrating sample magnetometer (VSM). The results show that as-prepared meso-SiO₂@Fe₃O₄(E) and meso-SiO₂@Fe₃O₄(C) microspheres, treated by acetone extraction and high temperature calcination, respectively, still maintain uniform core–shell structure with desirable mesoporous silica shell. Therein, the meso-SiO₂@Fe₃O₄(E) microspheres possess a distinct pore size distribution in 1.8–3.0 nm with large specific surface area (468.6 m²/g) and pore volume (0.35 cm³/g). Noteworthily, the coating period of this ultrasonic-assisted method (40 min) is much shorter than that of the conventional method (12–24 h). The morphology of microspheres and the mesoporous structure of silica shell are significantly influenced by initial concentration of CTAB (C_CTAB), ultrasonic irradiation power (P) and ultrasonic irradiation time (t). The acceleration roles of ultrasonic irradiation take effect during the whole coating process of mesoporous silica shell, including hydrolysis-condensation process of TEOS, co-assembly of hydrolyzed precursors and CTAB, and deposition of silica oligomers. In addition, the use of ultrasonic irradiation is favorable for improving the homogeneity of silica shell and the monodispersity of meso-SiO₂@Fe₃O₄ microspheres.     

Ultrasonic-assisted synthesis of the nanostructures of a Co(II) metal organic framework as a highly sensitive fluorescence probe of phenol derivatives

Nanostructures of a metal-organic framework with chemical formula, [Co(BDC)(L*)]_n.DMF (TMU-40), BDC = 1,4-benzendicarboxylate, L* = 5,6-dipyridin-4-yl-1,2,3,4-tetrahydropyrazine, under ultrasonic irradiation at ambient temperature and atmospheric pressure were prepared and characterized by Fourier-transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). Sonication time, concentration of initial reagents and ultrasonic generator power effects on the size and morphology of nano-structured compounds were studied. TMU-40 (for Tarbiat Modares University) displayed a good potential as a luminescent sensor against phenol derivatives consist of phenol, 4-aminophenol, 4-methylphenol and 4-chlorophenol. Nano-sized TMU-40 showed the better sensing performance in comparison to its bulk phase. The nano TMU-40 displayed very selective and sensitive in detection of phenol derivatives. The detection limit amounts of 15 nM and 63 nM were achieved for 4-aminophenol in nano TMU-40 and bulk TMU-40, respectively. The special structure and fluorescent character of L* ligand and high surface area of nano MOF provide an effective interaction between MOF and phenolic analytes to selectively and sensitively detect of the analyte molecules.     

Impedance spectroscopic studies of an organic semiconductor device incorporating a thin film of highly doped ZnPc with MoO3

We use experimental results of low signal impedance spectroscopy to investigate the conduction mechanism in organic semiconductor, zinc phthalocyanine (ZnPc). The first 10 nm, of a total of 150 nm thermally deposited ZnPc, was doped with molybdenum oxide (MoO₃) by co-evaporation to obtain a 20% doping concentration. The ac electrical parameters were measured at room temperature in the dc bias and frequency ranges of 0–5 V and 100 Hz–0.1 MHz, respectively. The variation of bulk resistance with applied bias presents a clear indication of space charge limited conduction in the fabricated device. The experimental results show a strong frequency dependence of capacitance and loss tangent at low frequencies and high applied bias, while at higher frequencies and low applied bias a weak dependence is observed. Moreover, the ac conductivity shows a strong dependence on frequency and is found to vary as ω^s with the index s≤1.15 suggesting a dominant hopping mechanism of conduction.     

The synthesis of hollow CdS nanospheres packed with square subunits

Hollow CdS nanospheres packed with square subunits were fabricated via microwave irradiation and pentaerythriol. The products were characterized with XRD, TEM, HRTEM, EDX and UV–vis spectrum. The results indicate that pentaerythriol is necessary in the formation of square subunits with high degree of crystallinity. A possible growth mechanism was proposed.     

Thermal conductivity of K0.3MoO3

Measurements of thermal conductivity of the blue bronze K_0.3MoO₃ are reported in the range 90–300K. A large anomaly at 183 K ascribed to the CDW transition and an overall good agreement of the experimental results with the estimations based on the Wiedemann-Franz are found.     

Ultrasonic-assisted synthesis of lignin-capped Cu2O nanocomposite with antibiofilm properties

Under ultrasonication, cuprous oxide (Cu₂O) microparticles (<5 µm) were fragmented into nanoparticles (NPs, ranging from 10 to 30 nm in diameter), and interacted strongly with alkali lignin (Mw = 10 kDa) to form a nanocomposite. The ultrasonic wave generates strong binding interaction between lignin and Cu₂O. The L-Cu nanocomposite exhibited synergistic effects with enhanced antibiofilm activities against E. coli, multidrug-resistant (MDR) E. coli, S. aureus (SA), methicillin-resistant SA, and P. aeruginosa (PA). The lignin-Cu₂O (L-Cu) nanocomposite also imparted notable eradication of such bacterial biofilms. Experimental evidence unraveled the destruction of bacterial cell walls by L-Cu, which interacted strongly with the bacterial membrane. After exposure to L-Cu, the bacterial cells lost the integrated structural morphology. The estimated MIC for biofilm inhibition for the five tested pathogens was 1 mg/mL L-Cu (92 % lignin and 8 % Cu₂ONPs, w/w %). The MIC for bacterial eradication was noticeably lower; 0.3 mg/mL (87 % lignin + 13 % Cu₂ONPs, w/w %) for PA and SA, whereas this value was appreciably higher for MDR E. coli (0.56 mg/mL, 86 % lignin and 14 % Cu₂O NPs). Such results highlighted the potential of L-Cu as an alternative to neutralize MDR pathogens.     

Controlled synthesis of gold nanospheres and single crystals in hydrogel

Narrow-dispersed gold nanospheres, regular single-crystal nanoplates and nanobulks were prepared, respectively, by reducing HAuCl₄ within a hydrogel system under UV irradiation. The formation of gold products with different geometric shape and size was found to depend on both the microenvironment of the gel matrix and the initial concentration of HAuCl₄. The resultant gold particles were investigated by UV–vis spectroscopy, X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and energy-dispersion X-ray spectroscopy. Electronic Supplementary Material The online version of this article at (doi: ) contains supplementary material, which is available to authorised users.     

基于MoO3/Ag/MoO3透明阳极的顶发射OLED的模拟计算与制备

运用传输矩阵法和正交分析法模拟计算出MoO₃/Ag/MoO₃透明电极的最佳厚度,采用镀膜实验验证模拟计算的准确性,制备了一系列不同MoO₃膜厚度和Ag膜厚度的透明电极。然后,制备了一系列顶发射有机电致发光器件:铝/氟化锂(LiF)/三(8-羟基喹啉)铝(Alq₃)/N,N'-二苯基-N,N'-(1-萘基)-1,1'-联苯-4,4'-二胺/三氧化钼(MoO₃)/银(Ag)/三氧化钼(MoO₃),来进一步验证模拟计算运用在器件制备中的准确性。MoO₃(10 nm)/Ag(10 nm)/MoO₃(25 nm)在532 nm处的透射率达到最大值88.256%,以该透明电极制备的器件与参考器件相比,性能有了明显提高,最大亮度和最大效率分别为20 076 cd/m²和4.03 cd/A,提高了18.5%和56%。器件性能的提高归因于顶发射OLED器件透射率的提高和MoO₃对空穴注入能力的提升。     

Solid-state synthesis and fluorescence properties of micron Bi2MoO6:Eu3+/C3N4 composite phosphors

The red emitting composite phosphors Bi₂MoO₆:Eu³⁺/C₃N₄ were prepared via a solid-state method and characterized by different techniques like XRD, SEM, FT-IR, Raman, UV-vis DRS and PL. The effects of reaction temperature and C₃N₄ amount on the structure and optical properties of Bi₂MoO₆ were studied in detail. The powder X-ray diffraction patterns showed that the crystal phase structure changed with the increase of temperature. Also, the introduction of C₃N₄ had a significant impact on photoluminescence properties, which provides a universal strategy for phosphors to improve luminescence performance.     

Low temperature coloration of WO3 and MoO3 thin films

The nature of the optical absorption band arising in amorphous MoO₃ and WO₃ films on insertion of hydrogen atoms was investigated carrying out this process over a wide temperature range. Hydrogen atoms were inserted in oxide films detached under the action of light from organic molecules adsorbed on the oxide surface. The absorption spectra were successfully fitted with three Gaussian functions each being assigned to the definite type of color centers. Paper presented at the 5th Euroconference on Solid State Ionics, Benalmádena, Spain, Sept. 13–20, 1998.