A facile and flexible process of β-cyclodextrin grafted on Fe3O4 magnetic nanoparticles and host-guest inclusion studies

In this study, a kind of novel surface-functionalized magnetic nanoparticles was fabricated by the Fe₃O₄ nanoparticles surface modification with mono-6-deoxy-6-(p-tolylsulfonyl)-cyclodextrin (6-TsO-β-CD), which were employed to interact with uric acid and their behavior was investigated by electrochemical methods. The architecture has been characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA), which confirmed that cyclodextrins have been effectively functionalized on the surface of Fe₃O₄ nanoparticles. The analyses of vibration sample magnetometer (VSM) verified that the nanoparticles owned good magnetic property. The grafted β-cyclodextrin on the Fe3O4 nanoparticles contributed to as a modified electrode for detecting uric acid with cyclic voltammograms. Electrochemical results revealed that the new materials could exhibit excellent molecules recognition ability and show high electrochemical response. The new nanoparticles simultaneously had unique properties of magnetic nanoparticles and cyclodextrins through combining their individual distinct advantages.     

Synthesis and characterization of ZrO2/MnO2/carbon clusters nanocomposite materials

Nano-sized ZrO₂/MnO₂/carbon clusters composite materials has been successfully obtained by the calcination of a Zr(acac)₄/Mn(acac)₃/epoxy resin complex under an oxygen atmosphere. The compositions of the resulting composite materials were determined using inductively coupled plasma (ICP) spectroscopy, elemental analysis and surface characterization by X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM). The ultraviolet–visible (UV–VIS), X-ray photoelectron spectra (XPS) and electron spin resonance (ESR) spectra of the composites were also measured. ESR spectral examinations suggest the possibility of an electron transfer in the process of MnO₂ → carbon clusters → ZrO₂. The visible light-responsive oxidation–reduction ability of the calcined material was also investigated.     

Optical and photocatalytic properties of novel heterogeneous PtSe2–graphene/TiO2 nanocomposites synthesized via ultrasonic assisted techniques

Novel material PtSe₂–graphene/TiO₂ nanocomposites were successfully synthesized through a facile ultrasonic assisted method. The prepared composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) with an energy dispersive X-ray (EDX),transmission electron microscopy (TEM), Raman spectroscopic analysis, UV–vis absorbance spectra and UV–vis diffuse reflectance spectra (DRS) analysis were obtained. The catalytic behavior was investigated through the decomposition of rhodamine B (Rh.B) as a standard dye. Enhanced photocatalytic activities were observed by increasing the weight% of graphene in the PtSe₂–graphene/TiO₂ nanocomposites. We observed that the coupling of TiO₂ with PtSe₂–graphene alter the optical properties by observing a precise band gap in the visible range.     

Impact of γ-rays on constructional,optical and thermal behavior of alkaline and non alkaline low density polyethylene

ABSTRACT

In this study, we investigated the graft copolymerization of methyl methacrylate (MMA) onto low-density polyethylene (LDPE) in the presence of aniline as an inhibitor by gamma radiation. An alkaline treatment was carried out for the prepared graft copolymer. The structural properties of the prepared samples were examined via X-ray diffraction (XRD) and scanning electron microscopy (SEM). The XRD peaks were slightly shifted, indicating an interaction between MMA and the polyethylene matrix. The morphology of the samples confirmed the homogenous grafted phase scattered onto the LDPE surface. Analysis of the absorption spectra indicated an allowed indirect transition mechanism. The Urbach energy (E_U) results showed that the value of the E_U for grafted LDPE was found to be higher than that of pure LDPE—up to 15?kGy irradiation dose, although this value decreases upon grafting. However, the value of the E_U for alkaline-treated grafted films decreases systematically by increasing the degree of grafting. The thermogravimetric analysis (TGA) of the sample indicated that the thermal stability of LDPE samples is significantly changed by grafting MMA onto it. Horowitz and Metzger's models were utilized to measure the activation energy of the thermal decomposition of all samples.     

Uniform design and regression analysis of LPCVD boron carbide from BCl3-CH4-H2 system

Boron carbide was prepared by low pressure chemical vapor deposition (LPCVD) from BCl₃-CH₄-H₂ system. The deposition process conditions were optimized through using a uniform design method and regression analysis. The regression model of the deposition rate was established. The influences of deposition temperature (T), deposition time (t), inlet BCl₃/CH₄ gas ratio (δ), and inlet H₂/CH₄ gas ratio (θ) on deposition rate and microstructure of the coatings were investigated. The optimized deposition parameters were obtained theoretically. The morphologies, phases, microstructure and composition of deposits were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman micro-spectroscopy, transmission electron microscopy (TEM), energy dispersive spectra (EDS), and Auger electron spectra (AES), the results showed that different boron carbides were produced by three kinds of deposition mechanisms.     

Enhanced photoactivity of CuPp-TiO2 photocatalysts under visible light irradiation

Three novel porphyrins, 5,10,15-tri-phenyl-20-[4-(3-phenoxy)-propoxy]phenyl porphyrin, 5,15-di-phenyl-10,20-di-[4-(3-phenoxy)-propoxy]phenyl porphyrin and 5-phenyl-10,15,20-tri- [4-(3-phenoxy)-propoxy]phenyl porphyrin, and their corresponding copper(II) complexes were synthesized and characterized spectroscopically. The photocatalytic effects of TiO₂ samples impregnated with copper(II) porphyrins was investigated by photodegradation of 4-nitrophenol (4-NP) in aqueous solution under visible light. The photocatalysts were characterized by means of scanning electron microscopy (SEM), X-ray diffraction (XRD), UV-vis spectra and FT-IR spectra. The results indicated that CuPps were successfully loaded and interacted with the surface of TiO₂ microsphere, which is crucial to enhance the activity of the catalytic composite under visible light.     

Growth mechanism and photoluminescence of the SnO2 nanotwists on thin film and the SnO2 short nanowires on nanorods

SnO2 nanotwists on thin film and SnO2 short nanowires on nanorods have been grown on single silicon substrates by using Au-Ag alloying catalyst assisted carbothermal evaporation of SnO2 and active carbon powders.The morphology and the structure of the prepared nanostructures are determined on the basis of field-emission scanning electron microscopy(FESEM),transmission electron microscopy(TEM),selected area electronic diffraction(SAED),high-resolution transmission electron microscopy(HRTEM),x-ray diffraction(XRD),Raman and photoluminescence(PL) spectra analysis.The new peaks at 356,450,and 489 nm in the measured PL spectra of two kinds of SnO2 nanostructures are observed,implying that more luminescence centres exist in these SnO2 nanostructures due to nanocrystals and defects.The growth mechanism of these nanostructures belongs to the vapour-liquid-solid(VLS) mechanism.     

Controlled synthesis of CeO<Subscript>2</Subscript> nanoparticles using novel amphiphilic cerium complex precursors

Maleic anhydride was grafted by long-chain alcohols (1-hexadecanol, 1-octadecanol) to amphiphilic mono-L cis-butene dicarboxylates (L = hexadecyl, octadecyl), i.e., MAH, MAO, respectively. Subsequently, corresponding amphiphilic cerium complexes with these two mono-L cis-butene dicarboxylate ligands (Ce(L')₃, L'= MAH, MAO) were synthesized and behaved as the precursors to prepare CeO₂ nanoparticles for both of which can form nanosized micelle-like aggregates by special self-assembly in the wet chemical process. The nanoparticles were further characterized by Fourier transform-infrared spectroscopy (FTIR), Diffuse reflectance ultraviolet-visible spectra (DRUVS), scanning electron microscope (SEM), transmission electron microscope (TEM), and x-ray diffraction (XRD). Both the CeO₂ nanoparticles are in a cubic fluorite structure and present regular and well-dispersion club-like morphology with average particle size in the range of 40–70 nm. Besides, the strong ultraviolet–visible absorption for these CeO₂ nanoparticles can be found at the long-wavelength ultraviolet to visible region of 200–500 nm.     

Surface-modified mesoporous silica with ferrocene derivatives and its ultrasound-triggered functionality

Novel ferrocene derivatives designed as gatekeepers were successfully composed on the pore outlet of amino-functionalized mesoporous silica by post-synthesis grafting where the peptide bond of the amine group (-NH₂) of mesoporous silica was linked with the carboxylic acid group (-COOH) of both ends of the ferrocene derivatives. The materials of the amine-functionalized mesoporous silica (NH₂-MS) and ferrocene-functionalized mesoporous silica (Fc-CONH-MS) were characterized using X-ray diffractions (XRD), Fourier-transform infrared (FT-IR), N₂ sorption isotherms, solid-state NMR spectra, scanning electron microscopy (SEM), energy dispersive X-ray (EDX), transmission electron microscopy (TEM), and UV-vis absorption spectra. The ferrocene attached to the mesoporous silica pore outlet was cleavaged by ultrasound irradiation, which opened the closed-pore outlets, suggesting a possible application for controlled release drug carrier.     

Surface-initiated atom transfer radical polymerization from TiO2 nanoparticles

Two kinds of hydrophilic polymers, poly(oxyethylene methacrylate) (POEM) and poly(styrene sulfonic acid) (PSSA), were grafted from TiO₂ nanoparticles via the surface-initiated atom transfer radical polymerization (ATRP) technique. Chlorine modified TiO₂ nanoparticles (TiO₂-Cl), the ATRP initiators, were synthesized by the reaction of -OH in TiO₂ with 2-chloropropionyl chloride (CPC). FT-IR, UV-vis spectroscopy and X-ray photoelectron spectroscopy (XPS) clearly showed that the polymer chains were successfully grafted from the surface of TiO₂ nanoparticles. The hydrophilically modified TiO₂ nanoparticles have a better dispersion in alcohol than unmodified nanoparticles, as revealed by transmission electron microscopy (TEM). It was also found that the polymer grafting did not significantly alter the crystalline structure of the TiO₂ nanoparticles according to the X-ray diffraction (XRD) patterns. Grafting amounts were 10% of the weight for both TiO₂-POEM and TiO₂-PSSA nanoparticles, as determined by thermogravimetric analysis (TGA).     

Synthesis and characterization of TiO2/MoO3/carbon clusters composite material

Nano-sized TiO₂/MoO₃/carbon clusters composite material has been successfully obtained by the calcinations of a TiO(acac)₂/MoO₂(acac)₂/epoxy resin complex under an oxygen atmosphere. The compositions of the resulting composite materials were determined using inductively coupled plasma (ICP) spectroscopy, elemental analysis and surface characterization by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The ultraviolet–visible (UV–Vis), X-ray photoelectron spectra (XPS) and electron spin resonance (ESR) spectra of the composites were also measured. ESR spectra of the composite materials suggest that they have visible light-responsive catalytic ability with an electron transfer process of carbon clusters → MoO₃ → carbon clusters → TiO₂.     

Some new 4‐coordinated nanostructure cadmium imidazolidine Schiff base complexes: Thermal behavior,antimicrobial, and DNA cleavage potential

In this study, a new series of cadmium halide/pseudohalide complexes with a novel Schiff base ligand containing imidazolidine ring has been successfully synthesized. The structure of the ligand and its complexes was characterized by analysis tools such as Fourier transform infrared, UV‐visible, proton and carbon nuclear magnetic resonance spectra, molar conductance, and thermal analysis. Also cadmium bromide and iodide nanostructure complexes have been prepared via sonochemical method. X‐ray powder diffraction and scanning electron microscopy techniques confirmed nanostructure sheets for these 2 cadmium complexes. All the newly prepared compounds were screened for their antimicrobial activities, against 4 bacterial and 2 fungal strains using disk diffusion and serial dilution methods. The CdL(N₃)₂ and CdLCl₂ complexes showed the best antimicrobial activity as compared with other compounds. Moreover, DNA cleavage potential of all compounds was investigated by agarose gel electrophoresis method. The results showed remarkable ability of some cadmium complexes for DNA cleavage. Furthermore, thermal behaviors of all cadmium complexes were studied in the range of room temperature to 800°C under nitrogen atmosphere. The complexes were thermally decomposed via 2 to 4 steps. Cadmium metal was suggested as final residue at the end of thermal decomposition process.     

A simple sonochemical approach for synthesis and characterization of Zn2SiO4 nanostructures

Zn₂SiO₄ nanoparticles have been successfully prepared via a simple sonochemical method, for the first time. The effect of various parameters including ultrasonic power, ultrasonic irradiation time and different surfactants were investigated to reach optimum condition. The as-prepared nanostructures were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmittance electron microscopy (TEM), Fourier transform infrared (FT-IR) spectra and energy dispersive X-ray microanalysis (EDX). The photocatalytic activity of Zn₂SiO₄ nano and bulk structures were compared by degradation of anionic dye methyl orange in aqueous solution under UV-light irradiation. Moreover, the cyclic voltammetry analysis of Zn₂SiO₄ nano and bulk structures were investigated.     

Supercritical fluid-assisted synthesis of a carbon nanotubes-grafted biocompatible polymer composite

A nanocomposite consisting of multi-wall nanotubes (MWNTs) grafted with a biocompatible polymer poly(2-hydroxyethyl methacrylate) was prepared by in situ polymerization in supercritical carbon dioxide. The surface of the MWNTs was first surface modified with hydroxyl groups in the solution of KMnO₄ and a phase-transfer catalyst. MWNT-OH was then functionalized with vinyl groups using a silane coupling agent, γ-methacryloxypropyltrimethoxysilane. The silane groups can improve the dipersion of MWNTs in supercritical carbon dioxide, while the terminal vinyl groups help fabricate polymer chains on the MWNT surface. The as-synthesized products were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and thermo-gravimetric analysis. The SEM and TEM images showed that the nanotubes were well coated with the polymer shell. The composite had higher thermal stability than the pure polymer and dispersed well in methanol. This biocompatible polymer composite was prepared using a green method and is expected to be useful as a biomaterial composite with potential applications in the biological field.     

Direct synthesis and characterization of phenyl-functionalized SBA-15

Phenyl-functionalized SBA-15 materials (Ph-SBA-15) were directly synthesized by using tri-block copolymer Pluronic P123 as templating agent under acidic conditions. The samples were characterized by Fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), thermogravimetry analysis (TGA) and N₂ adsorption-desorption. The results show that the phenyl groups are covalently attached to the pore wall of SBA-15 after modification. The functionalized materials still preserve a desirable two-dimensional P6mm hexagonal structure and have large specific surface area and pore volume although the molar ratio of phenyltrimethoxysilane in total silica precursors is as high as 23.0%.     

Sol–gel synthesis of 8 nm magnetite (Fe3O4) nanoparticles and their magnetic properties

Magnetite (Fe₃O₄) nanoparticles were successfully synthesized by a sol–gel method. The obtained nanoparticles were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive analysis by X-ray (EDAX), transmission electron microscopy (TEM), superconducting quantum interference device (SQUID) and Mössbauer spectrometry. XRD and Mössbauer measurements indicate that the obtained nanoparticles are single phase. TEM analysis shows the presence of spherical nanoparticles with homogeneous size distribution of about 8 nm. Room temperature ferromagnetics behavior was confirmed by SQUID measurements. The mechanism of nanoparticles formation and the comparison with recent results are discussed. Finally, the synthesized nanoparticles present a potential candidate for hyperthermia application given their saturation magnetization.     

Synthesis of fluorinated TiO2 hollow microspheres and their photocatalytic activity under visible light

Fluorinated TiO₂ hollow microspheres with three-dimensional hierarchical architecture were prepared by solvothermally treatment using solid microspheres as precursor. The obtained solid and hollow TiO₂ microspheres were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET), X-ray photoelectron spectroscopy (XPS), UV-Vis diffuse reflectance spectrum (DRS) and photoluminescence (PL) spectra. The photocatalytic activity of as-prepared solid and hollow TiO₂ microspheres was determined by degradation of methyl orange (MO) under visible light irradiation. The results showed that the surface fluorination, the existence of accessible mesopores channels, and the increased light harvesting abilities could remarkably improve the photocatalytic activity of TiO₂ hollow microspheres.     

Structure and photocatalytic properties of copper-doped rutile TiO2 prepared by a low-temperature process

Copper-doped titania with variable Cu/Ti ratios have been prepared via a simple aqueous-phase method at 85 °C. The obtained products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and UV-vis absorption spectra analysis. The photocatalytic properties of the products were tested by photocatalytic degradation of aqueous brilliant red X-3B solution. The results showed that the sample with 2% copper doping has the best photocatalytic activity, which is 3 times that of undoped rutile titania. The effect of the doped copper on the structure and property of TiO₂ has also been discussed.     

Synthesis of ZnS nanorods by annealing precursor ZnS nanoparticles in NaCl flux

ZnS nanorods were fabricated by annealing precursor ZnS nanoparticles, which were prepared by one-step, solid-state reaction of ZnCl₂ and Na₂S through grinding by hand at ambient temperature, in NaCl flux. The as-prepared ZnS nanorods have diameters of 40-80 nm, and lengths up to several micrometers. The structural features and chemical composition of the nanorods were investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution transmission electron microscopy (HRTEM), and Raman spectra.     

Time-dependent growth of crystalline Au0-nanoparticles in cyanobacteria as self-reproducing bioreactors: 1. Anabaena sp.

In the experiments, multifunctional nanocomposites with fluorescence, superparamagnetism, and bioactivity were synthesized to isolate and detect bacteria. Fluorescent-magnetic nanocomposites (FMNPs) (Fe₃O₄@SiO₂@FITC–SiO₂, core/shell) were first synthesized. Then, FMNPs were conjugated with N-hydroxysuccinimide-activated 4-oxo-4-(prop-2-ynyloxy) butanoic acid (NHS-activated ester) by the linker of 3-aminopropyltriethoxysilane, and alkyne-functionalized fluorescent-magnetic nanocomposites (FMNPs-alkyne) were produced. After 3′-azidopropyl-O-α-d-manno-pyranoside was grafted on the surface of FMNPs-alkyne by click chemistry, the final product—mannose derivatives-grafted fluorescent-magnetic nanocomposites (FMNPs-mannose) were obtained. Common techniques (Nuclear magnetic resonance, ESI mass spectra, etc.) indicated the successful synthesis of the target products. The results of scanning electron microscopy, transmission electron microscopy, and dynamic light scattering showed that FMNPs with one or more magnetic cores have regular structure with a diameter around 100 nm. Fluorescence spectra and fluorescence microscopy indicated that those nanocomposites exhibited strong and stable fluorescence property. FMNPs-mannose have a saturation magnization of 6.88 emu/g at room temperature. FMNPs-mannose were applied to adhere to Escherichia coli ATCC25722 and Staphylococcus aureus ATCC6538. The results showed that FMNPs-mannose were able to specifically adhere to E. coli ATCC25722. However, it had no effect with S. aureus ATCC6538. The obtained FMNPs-mannose will find its application in bacteria detection and separation.