Search results for "Selected area diffraction"
showing 10 items of 34 documents
Mesocrystalline Cr and Sb-codoped anatase visible-light-driven photocatalyst
2018
Abstract We report on the synthesis, characterization and visible-light-driven photocatalytic activity of mesocrystalline Cr- and Sb-codoped anatase nanoparticles. Discrete and morphologically well-defined assemblies of anatase nanoparticles sized below 100 nm × 50 nm were prepared by hydrothermal aging of aqueous solutions containing titanium alkoxide, chromium acetylacetonate, antimony acetate and triethanolamine (TEOA) as stabilizer. The as-prepared and TEOA-free doped nanoparticles showed similar crystallographic parameters and spectroscopic features. The incorporation of Cr and Sb dopant cations into the anatase nanoparticles was evaluated by Rietveld refinement of X-ray diffraction pa…
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 …
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–…
Consolidation and protection by nanolime: recent advances for the conservation of the graffiti, Carceri dello Steri Palermo and of the 18th century l…
2014
Abstract Nanolime dispersed in 2-propanol was extensively used for the consolidation of wall paintings. The knowledge of the advances of this methodology dealing with all the possible effects associated with the nanolime new material in conservation is fundamental to assess and improve the technique. In this paper, four different dispersions of Ca(OH) 2 nanoparticles were characterised by Small Angle X-rays Scattering technique (SAXS) and Transmission Electron Microscopy (TEM) in order to achieve information on size, shape, polydispersity, agglomeration, and crystal structure (by SAED patterns) of the particles. Once characterised, the dispersions were tested in two different case studies, …
H-bonding schemes of di- and tri-p-benzamides assessed by a combination of electron diffraction, X-ray powder diffraction and solid-state NMR
2010
The crystal structures of di- and tri-p-benzamides are solved by a combination of single crystal, electron and powder X-ray diffraction. Different hydrogen-bonding schemes observed in the two structures are described and classified. The hydrogen-bonding networks are correlated to complementary data obtained from multinuclear solid-state NMR.
Growth and characterization of self-assembled Cd1−xMgxO (0 ≤ x ≤ 1) nanoparticles on r-sapphire substrates
2014
In this work, the growth of isolated Cd1−xMgxO nanoparticles on r-sapphire substrates is extended to the entire range of Mg content (0 ≤ x ≤ 1) using the spray pyrolysis method. The sizes of the Cd1−xMgxO nanoparticles were in the ranges 4–6 nm and 15–30 nm (with a nanoparticle density of 1010 cm−2). The composition of the nanoparticles was determined using transmission electron microscopy energy dispersive X-ray analysis (TEM-EDAX), while the compound formation was confirmed using X-ray photoelectron spectroscopy. A systematic decrease in the a lattice parameter of Cd1−xMgxO on increasing the Mg content substantiated the successful incorporation of Mg2+ ions into the cubic CdO lattice. Sin…
Facile Large Scale Synthesis of WS2 Nanotubes from WO3 Nanorods Prepared by a Hydrothermal Route.
2005
Abstract Hexagonal WO 3 nanorods of 5–50 nm in diameter and 150–250 nm in length have been synthesised in gram quantities by a low temperature hydrothermal route using citric acid as a structural modifier and hexadecylamine as a templating agent. The ratio of [A]/[W] play an important role on WO 3 nanorods formation. These WO 3 nanorods were found highly suitable as a precursor for the synthesis of a good yield of multiwalled WS 2 nanotubes by reducing them with H 2 S at 840 °C for 30 min. The length and the wall thickness of the WS 2 nanotubes could be altered by controlled reduction of the oxide precursor. The morphology, structure and the composition of the WO 3 nanorods and WS 2 nanotub…
Synthesis and characterization of ZnO nano and micro structures grown by low temperature spray pyrolysis and vapor transport.
2012
In this work we present a systematic study of ZnO micro and nanostructures grown by spray pyrolysis (SP) and by physical vapour transport (PVT) on glass and c-sapphire substrates at low temperatures. Optimised growth conditions have allowed to obtain homogeneous ZnO nanolayers composed of quasi-spherical nanoparticles in the range 2 to 8 nm by spray pyrolysis, while by PVT the selected growth conditions allow to produce a wide variety of morphologies (tripods, grains, arrows and wires) of nano and microsize dimension. Grazing incidence X-ray diffraction, field emission scanning electron microscopy (FE-SEM), high resolution transmission electron microscopy (HRTEM), selected area electron dif…
Towards automated diffraction tomography: Part I—Data acquisition
2007
Abstract The ultimate aim of electron diffraction data collection for structure analysis is to sample the reciprocal space as accurately as possible to obtain a high-quality data set for crystal structure determination. Besides a more precise lattice parameter determination, fine sampling is expected to deliver superior data on reflection intensities, which is crucial for subsequent structure analysis. Traditionally, three-dimensional (3D) diffraction data are collected by manually tilting a crystal around a selected crystallographic axis and recording a set of diffraction patterns (a tilt series) at various crystallographic zones. In a second step, diffraction data from these zones are com…
Structure analysis of titanate nanorods by automated electron diffraction tomography
2011
A hitherto unknown phase of sodium titanate, NaTi3O6(OH)·2H2O, was identified as the intermediate species in the synthesis of TiO2 nanorods. This new phase, prepared as nanorods, was investigated by electron diffraction, X-ray powder diffraction, thermogravimetric analysis and high-resolution transmission electron microscopy. The structure was determined ab initio using electron diffraction data collected by the recently developed automated diffraction tomography technique. NaTi3O6(OH)·2H2O crystallizes in the monoclinic space group C2/m. Corrugated layers of corner- and edge-sharing distorted TiO6 octahedra are intercalated with Na+ and water of crystallization. The nanorods are typically …