Search results for "Spectroscopy"

Preparation and characterisation of TiO2 (anatase) supported on TiO2 (rutile) catalysts employed for 4-nitrophenol photodegradation in aqueous medium…

1999

Abstract In this paper the preparation of two sets of polycrystalline photocatalysts prepared by supporting TiO2 (anatase) on TiO2 (rutile) or Al2O3 is reported. The powders were prepared by a wet impregnation method using titanium(IV) isopropylate. The impregnation was followed by thermal treatment and this procedure was repeated several times in order to obtain samples with progressively increasing amounts of TiO2 (anatase). The photocatalytic activity of all of the specimens was tested by carrying out the 4-nitrophenol photodegradation, used as a “probe” reaction, in aqueous medium and in different kinds of batch photoreactors. The solids were characterised by X-ray diffraction (XRD), sp…

Nanostructured Pt–TiO2 composite thin films obtained by direct liquid injection metal organic chemical vapor deposition: Control of chemical state by…

2015

Abstract Nanostructured Pt–TiO 2 composite thin films were synthesized by direct liquid injection metal organic chemical vapor deposition process, using trimethyl(methylcyclopentadienyl)platinum and titanium isopropoxide as precursors. Surface and cross-sectional morphologies obtained by scanning electron microscopy and transmission electron microscopy evidenced the uniform distribution of platinum nanoparticles in the TiO 2 matrix. At higher Pt content, the X-ray diffraction analysis showed that the face-centered cubic phase of platinum appeared together with an anatase TiO 2 structure. In addition, as far as the platinum chemical state is concerned, the co-deposition of TiO 2 and Pt allow…

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…

Influence of Amorphous TiO2-x on Titania Nanoparticle Growth and Anatase-to-Rutile Transformation

2012

Amorphous TiO2-x formed together with precursors and anatase nuclei, during TiCl4 hydrolysis at soft conditions, influences both crystal growth and phase stability. The highly defective nanoparticles of anatase grow by reaction of their basic hydroxyls with acidic ones of TiO2 precursor species. The growth of anatase crystals, however, is affected by their interactions with simultaneously formed amorphous TiO2-x which increasingly covers the particles hindering the anatase-precursor contact. The interactions among anatase and amorphous and precursor components have been studied by H-1-MAS (magic angle spinning) NMR spectroscopy. The interaction between acid and basic hydroxyls favors the fo…

Preparation characterization and photocatalytic activity of polycrystalline ZnO/TiO2 systems. 2. Surface, bulk characterization, and 4-nitrophenol ph…

2001

Electron spin resonance spectroscopy (ESR), Fourier transform infrared spectroscopy (FTIR), and monitoring of pyridine (py) and boric acid trimethyl ester (BATE) adsorption for determining surface acidity and basicity, respectively, were used to carry out further characterization of mixed ZnO/TiO2 polycrystalline solids prepared by different methods. Moreover, the powders were tested in a batch photoreactor for a probe reaction, i.e., 4-nitrophenol photodegradation in aqueous medium. ESR results indicated the presence of signals attributable to Zn+ species in ZnO/TiO2 (anatase) solids, while in ZnO/TiO2 (rutile) samples the presence of zinc induced only the formation of signals probably due…

Preparation characterization and photocatalytic activity of polycrystalline ZnO/TiO2 systems. 1. Surface and bulk characterization

2001

Polycrystalline ZnO/TiO2 solids have been prepared with four different methods using home prepared TiO2 (anatase) or TiO2 (rutile) as supports and Zn(NO3)2·6H2O or Zn(CH3COO)2·2H2O as precursors for ZnO. The bulk and surface properties of the samples were investigated by means of TG-DTA, XRD, TEM, SEM-EDAX, XPS, BET surface area determination, and porosity measurements. XRD and TEM results indicate that no significant defect structures exist in any of the samples. The ZnO crystallinity and its enrichment on the surface of TiO2 particles were dependent on the preparation method. The surface areas generally decrease by increasing the amount of ZnO except when ZnO from Zn(CH3COO)2·2H2O was sup…

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 …

2018

We report a novel multi-step method for the preparation of ordered mesoporous titania scaffolds and show an illustrative example of their application to solar cells. The method is based on (monolayer) colloidal nanosphere lithography that makes use of polystyrene nanoparticles organised at a water–air interface and subsequently transferred onto a solid substrate. A titania precursor solution (titanium(IV) isopropoxide in ethanol) is then drop-cast onto the monolayer and left to “incubate” overnight. Surprisingly, instead of the expected inverse monolayer-structure, a subsequent calcination step of the precursor yields an ordered monolayer of hollow titania nanospheres with a wall thickness …

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–…

Photoelectrochemical characterization of anatase-rutile mixed TiO2 nanosponges

2016

This work studies the influence of using hydrodynamic conditions during anodization on the morphology and electrochemical properties of anatase/rutile mixed TiO2 nanotubes (Reynolds number, Re = 0) and nanosponges (Re > 0). To this purpose different techniques were used, such as: microscopy techniques (Field-Emission Scanning Electron Microscope, FE-SEM, and Confocal Laser-Raman Spectroscopy), Electrochemical Impedance Spectroscopy (EIS), Mott Schottky (MS) analysis and photoelectrochemical water splitting tests. This investigation demonstrates that the morphology of TiO2 nanostructures may be greatly affected due to the hydrodynamic conditions and it can be adjusted in order to increase th…