Search results for "ELECTRON MICROSCOPY"
showing 10 items of 706 documents
Anatase nanoparticles boundaries resulting from titanium tetrachloride hydrolysis
2017
An important factor that governs solar energy transformation into electrical or chemical energy, when using nanoparticles-based devices, is the spatial location of traps limiting electron transport. Evidences have been presented indicating that the electron diffusion is strongly influenced by nanoparticle boundaries, whose characteristics depend on the particles preparation. In the present work we have studied the role of hydrated excess proton structures in the formation of anatase nanoparticles boundaries in samples prepared by TiCl4 hydrolysis at low temperature and strong acidic conditions. The samples, constituted by anatase nanocrystals but, mainly, by amorphous titania, are studied b…
The effect of the surface disordered layer on the photoreactivity of titania nanoparticles
2017
It is well known that the surface of metal oxide catalysts presents, usually, non-crystalline species containing impurities and low coordinated cations, which are observed in HRTEM images as a disordered layer of amorphous phase. Despite of being these species more accessible and less stable than the crystalline catalysts components, they have been rarely considered when analysing the catalyst activity. In this work, we have studied the effect of a treatment with HCl solution at pH = 0 on the characteristics of the disordered layer in two commercial anatase TiO2 samples, using techniques such as TGA, 1H MAS-NMR and HRTEM, and by determining these sample photocatalytic activity for the 4-nit…
Mesocrystalline anatase nanoparticles synthesized using a simple hydrothermal approach with enhanced light harvesting for gas-phase reaction
2018
Mesocrystalline TiO2 nanoparticles were synthesized using a hydrothermal approach. A simple two-step procedure at low temperature (<140 °C) allowed the nucleation of primary particles sized 2–4 nm and their subsequent assembly as almost spherical aggregates sized ≈20 nm. X-ray powder diffraction (XRD), Raman and X-ray photoelectron spectroscopy (XPS) studies, and HRTEM studies confirmed anatase as the unique TiO2 crystalline phase. The mesocrystalline structure of the anatase aggregates was clearly evidenced by HRTEM and SAED results. The mesocrystalline nanopowders exhibit a mesoporous structure with a surface area and pore volume of 63.5 m2 g−1 and 0.22 cm3 g−1, respectively. Ultraviolet …
Polyacrylonitrile block copolymers for the preparation of a thin carbon coating around TiO2 nanorods for advanced lithium-ion batteries.
2013
Herein, a new method for the realization of a thin and homogenous carbonaceous particle coating, made by carbonizing RAFT polymerization derived block copolymers anchored on anatase TiO2 nanorods, is presented. These block copolymers consist of a short anchor block (based on dopamine) and a long, easily graphitizable block of polyacrylonitrile. The grafting of such block copolymers to TiO2 nanorods creates a polymer shell, which can be visualized by atomic force microscopy (AFM). Thermal treatment at 700 °C converts the polyacrylonitrile block to partially graphitic structures (as determined by Raman spectroscopy), establishing a thin carbon coating (as determined by transmission electron m…
Hydrothermal-mediated synthesis of orange Cr, Sb-containing TiO 2 nano-pigments with improved microstructure
2017
Abstract A hydrothermal-mediated via was developed to prepare discrete, non-aggregated Cr,Sb-doped rutile nano-pigments. After annealing the Cr- and Sb-containing TiO2 anatase nanocrystals obtained by hydrothermal aging the nano-pigments Cr,Sb-TiO2 were characterized with the aid of X-ray diffraction (XRD) including lattice parameter and crystallite size determination, Raman spectroscopy, field emission scanning and transmission electron microscopies (FESEM and TEM, respectively) including energy-dispersive X-ray (FESEM/EDX) spectroscopy, high resolution transmission electron microscopy (HRTEM) including selected area electron diffraction (SAED), ultraviolet–visible diffuse reflectance (UV–…
Phase formation in mixed TiO2-ZrO2 oxides prepared by sol-gel method
2011
Pure titania, zirconia, and mixed oxides (3—37 mol.% of ZrO2) are prepared using the sol-gel method and calcined at different temperatures. The calcined samples are characterized by Raman spectroscopy, X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, and nitrogen adsorption porosimetry. Measurements reveal a thermal stability of the titania anatase phase that slightly increases in the presence of 3—13 mol.% of zirconia. Practically, the titania anatase-rutile phase transformation is hindered during the temperature increase above 700 C. The mixed oxide with 37 mol.% of ZrO2 treated at 550 C shows a new single amorphous phase with a surface area of the…
High photodegradation and antibacterial activity of BN–Ag/TiO 2 composite nanofibers under visible light
2018
To develop material with good photocatalytic properties for organic compound degradation and bacterial removal, we produced Ag/TiO2 and BN–Ag/TiO2 composite nanofibers that included controlled amounts of boron nitride (BN) nanosheets and silver (Ag). After annealing at 500 °C under air, we used scanning electron microscopy, transmission electron microscopy, Brunauer–Emmet–Teller analysis, X-ray diffraction, energy-dispersive X-ray spectroscopy, Raman spectroscopy, UV-visible reflectance spectroscopy and room temperature photoluminescence to investigate the morphological, structural and optical properties of all samples. The photocatalytic tests using methylene blue under visible light, in r…
Influence of temperature on the synthesis of thiol-stabilized CdTe nanoparticles in aqueous solutions
2010
We have investigated the evolution of thiol-capped cadmium telluride nanocrystals prepared in aqueous solutions at low and room temperature followed by heating at 50–100 °C. The UV–visible absorption spectra, as well as transmission electron microscopy, atomic force microscopy, and dynamic light scattering observations made it possible to reveal differences in size and structure originating from different heating temperatures. It was shown that minimization of the nucleation process temperature provided formation of larger nanoparticles than at higher temperatures.
Facile synthesis and characterization of functionalized, monocrystalline rutile TiO2 nanorods.
2006
Functionalized, monocrystalline rutile TiO2 nanorods were prepared from TiCl4 in aqueous solution under acidic conditions in the presence of dopamine, followed by aging and hydrothermal treatment at 150 degrees C. The surface-bound organic ligand controls the morphology as well as the crystallinity and the phase selection of TiO2. The presence of monocrystalline rutile TiO2 was confirmed by X-ray powder diffraction and HRTEM investigations. The as-prepared nanorods are soluble in water at pH3. The surface functionalization was analyzed by IR and 1H NMR, confirming the presence of dopamine on the surface. The surface amine groups can be tailored further with functional molecules such as dyes…
Characterization of Zirconium Phosphate/Polycation Thin Films Grown by Sequential Adsorption Reactions
1997
Monolayer and multilayer thin films consisting of anionic α-zirconium phosphate (α-ZrP) sheets and polycations (poly(allylamine hydrochloride) (PAH), cytochrome c) were characterized by transmission electron microscopy (TEM), ellipsometry, UV−visible absorbance spectroscopy, reflectance FT-IR, XPS, and X-ray diffraction. Titration and powder X-ray diffraction experiments confirm that exfoliation of α-ZrP begins to occur when enough tetra(n-butylammonium) hydroxide (TBA+OH-) has been added to exceed single-layer packing of TBA+ ions (x ≈ 0.50) in the intercalation compound Zr(HPO4)2-x(TBA+PO4-)x·nH2O. The identical contrast of many sheets in TEM micrographs suggests that the suspension is un…