T. Siciliano

SEM-EDS investigation on PM10 data collected in Central Italy: Principal Component Analysis and Hierarchical Cluster Analysis

BackgroundPrincipal Component Analysis (PCA) and Hierarchical Cluster Analysis (HCA) were applied on PM10 particle data in order to: identify particle clusters that can be differentiated on the bases of their chemical composition and morphology, investigate the relationship among the chemical and morphological parameters and evaluate differences among the sampling sites. PM10 was collected in 3 different sites in central Italy characterized by different conditions: yard, urban and rural sites. The concentration of 20 chemical parameters (C, O, Na, Mg, Al, Si, P, Cd, Cl, K, Ca, Sn, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn) were determined by Scanning Electron Microscopy – Energy Dispersive X-ray Spectroscopy (SEM-EDS) and the particle images were processed by an image analysis software in order to measure: Area, Aspect Ratio, Roundness, Fractal Dimension, Box Width, Box Height and Perimeter.ResultResults revealed the presence of different clusters of particles, differentiated on the bases of chemical composition and morphological parameters (aluminosilicates, calcium particles, biological particles, soot, cenosphere, sodium chloride, sulphates, metallic particles, iron spherical particles). Aluminosilicates and Calcium particles of rural and urban sites showed a similar nature due to a mainly natural origin, while those of the yard site showed a more heterogeneous composition mainly related to human activity. Biological particles and soot can be differentiated on the bases of the higher loads of Fractal Dimension, which characterizes soot, and content of Na, Mg, Ca, Cl and K which characterize the biological ones. The soot of the urban site showed higher loadings of Roundness and Fractal Dimension than the soot belonging to the yard and rural sites, this was due to the different life time of the particles. The metal particles, characterized mainly by the higher loading of iron, were present in two morphological forms: spherical and angular particles. The first were generated by a fusion process at high temperature, while the second one had crustal origin (those characterized by typical terrigenous elements) and also human origin.ConclusionIn this work a protocol for the morphological-chemical characterization of single particles has been developed. SEM analysis allows to classify particles in 10 different families and PCA and HCA have provided information about the sources of PM and similarities and differences among the sites.

Physical properties of sputtered molybdenum oxide thin films suitable for gas sensing applications

Molybdenum oxide thin films were obtained by r.f. reactive sputtering of a molybdenum target. Optical and electrical characterization was performed in order to determine the energy gap and to investigate the electrical transport mechanism. In particular, electrical characterization showed that the transport properties of our thin films were governed by a scattering mechanism associated with the inter-grain barrier height. Finally, the analysis of the electrical behaviour of these films in controlled atmosphere allowed us to test the gas sensing properties, and to show that the conduction energy increased in the presence of electroactive gases.

Te oxide nanowires as advanced materials for amperometric nonenzymatic hydrogen peroxide sensing.

A new nonenzymatic platinum Te oxide nanowires modified electrode (Pt/TeO2-NWs) for amperometric detection of hydrogen peroxide (H2O2) is proposed. The modified electrode has been developed by direct drop casting, with TeO2 nanowires (TeO2-NWs), synthesized by thermal evaporation of Te(0) in an oxygen atmosphere. The morphological and spectroscopic characterization of the TeO2-NWs as synthesized on Pt foil was performed by scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) analysis. XPS and XRD analyses are especially involved to gain information on the chemical environment of TeO2-NWs in contact with Pt surface. Moreover electrochemical characterization of these new modified Pt/TeO2-NWs modified electrodes was performed by Cyclic Voltammetry (CV) and Cronoamperometry (CA) in phosphate buffer (pH=7; I=0.2) to investigate the sensing properties of this material against H2O2. The proposed sensor exhibits a wide linear and dynamic range from 2 µM to 16 mM (R(2)=0.9998) and the detection limit is estimated to be 0.6 µM (S/N=3). Moreover, this sensor shows a rapid amperometric response time of less than 5s and possessed good reproducibility. These results indicate that Pt/TeO2-NWs composite is suitable to be used as material for sensing applications.

X-Ray photoelectron spectroscopy characterisation of Langmuir–Blodgett films containing TiO2 nanoparticles grown by room-temperature hydrolysis of TiO(C2O4)22−

Abstract A new approach to the preparation of TiO2 nanoparticles embedded in organic films is described. This room-temperature method is based on a Langmuir–Blodgett standard procedure using an aqueous subphase in which TiO(C2O4)22− is dissolved. Spectroscopic investigations on the subphase show that TiO2 nanoparticles are dispersed in the solution. Careful X-ray photoelectron spectroscopy characterisation of Langmuir–Blodgett films reveals that those particles are transferred into the interior of the films during growth of the n-octadecylamine layers.

Modulation of charge transport in diamond-based layers

Doping of diamond by substitutional insertion of metallic species or production of diamond/metals nanocomposite layers has been obtained by a hybrid chemical vapor deposition based technique. The potential of such an approach makes it possible to obtain a wide class of purposely designed diamond-based structures characterized by specific properties of charge transport. Reflection high-energy electron diffraction, scanning electron microscopy and x-ray dispersive spectrometry have been used to study the structural and compositional characteristics of some Nd-, W- and Ti-containing diamond films. The peculiar electrical properties conferred to the host diamond layers by the insertion of various metals have been investigated in the range of 25–500 K by performing Hall effect and conductivity measurements. The mechanism of charge transport and the electrical properties of these materials are found to be mainly governed by organization of the metallic species, which can be in different forms, such as dispersio...