Amorphous silicon–nitrogen (a–Si1−xNx:H) alloys, thin films, and multilayers deposited by ultrahigh-vacuum plasma-enhanced chemical vapor deposition were studied and modeled by x-ray reflectivity (XRR) measurements. The analysis of XRR data obtained from the single-layer samples allowed us to calculate the density, thickness, and interface roughness of each layer. To check the deposition parameters, the deviation (tnom – texp)/(tnom) of the measured thickness texp from the nominal thickness tnom was evaluated. Based on these results, a simulation of a multilayer film, obtained by deposition alternating stoichiometric and substoichimetric layers was carried out. It is shown that the best fitting is obtained by introducing into the XRR calculation a thickness distribution with a standard deviation related to the deviation (tnom – texp)/(tnom) estimated for the single layers.

The effects of doping on the morphological and microstructural properties of TiO2 nanopowders produced by laser pyrolysis were investigated mainly by x-ray diffraction (XRD) and electron microscopy. Samples of TiO2 powders were prepared by doping with different trivalent cations (Al and Ga). The powders were calcined at different temperatures in the range 400–1000 °C for 18 h, as well as at constant T = 700 °C up to 160 h. After each thermal treatment, XRD patterns were collected. The analysis of XRD patterns allowed us to estimate the microstrains and average crystallite size and to observe the evolution of the microstructural parameters with temperature. Both Al and Ga inhibited the crystallite growth of TiO2 anatase and the rutile phases, this effect being larger in the Al-doped powders.

The kinetics of phase transitions and phase segregation induced by annealing temperature on the Ti–W–O gas-sensing layer was studied by x-ray diffraction, Raman spectroscopy, and scanning electron microscopy. The main goal was to identify, on the basis of kinetics studies, structurally stable Ti–WO3 thin film phases and compare their response to polluting gases in order to determine possible correlations between structural and electrical properties of the sensing layers.

A low cost and efficient method of doping pure zinc oxide powders for luminescence applications is presented. The powders have been obtained from pure, non-luminescent ZnO by thermally induced doping under a nitrogen flux and in the presence of ZnS powders. Structural characterization has been carried out by X-ray diffraction analysis (XRD), while luminescence properties have been studied with both a spectrofluorimeter and microraman spectrometer. Emission spectra have shown an increase of the luminescence with treatment temperature. The XRD patterns of all samples showed, along with reflections of the hexagonal phase of ZnO, other reflections ascribed to the hexagonal phase of ZnS. Upon further annealing in air at 800°C, the ZnS reflections disappear even though the luminescence still persists with a comparable intensity. Luminescence is ascribed to ZnO reduction due to the interaction of S with ZnO. It has also been observed that excitation with a He-Ne laser beam (λ=633 nm) with a high specific power (5×10−3 W·µm−2) yielded blue-green luminescence in spite of excitation below the band-to-band absorption threshold.

Rh nanoparticles supported on ZrO2 powder were prepared by adsorbing Rh4(CO)12 clusters from hexane solution under Ar atmosphere. Four samples with Rh content ranging from 0.25 Rh wt.% up to 4.10 Rh wt.% were studied by x-ray diffraction (XRD), transmission electron microscopy (TEM), x-ray photoelectron spectroscopy (XPS), scanning Auger microscopy (SAM), and time of flight secondary ion mass spectroscopy (ToF-SIMS). TEM measurements show, for all the samples, Rh particles with a size of about 50 Å. The 4.10 Rh wt.% sample also shows some agglomerates of Rh nanoparticles and only for this sample Rh metallic phase was detected by XRD. The profile analysis of the XRD lines indicates an average size of the Rh crystallites of about 60 Å. XPS studies show only a single spectral component for the Zr3d5/2 core line at 182.2 eV. Instead, at least, two components at 307.2 eV and 308.5 eV are detected for the Rh3d5/2 core line. These results suggest that Zr is present only as oxidized state, whereas nonoxidized and oxidized Rh are both observed. A nonoxidized Rh state is also suggested by the XPS valence band electron removal spectrum which exhibits a significant emission within the ZrO2 band gap assigned to Rh 4d bands. A further support to this finding arises from scanning Auger maps of OKVV and RH where nonoxidized Rh is observed. Finally scanning Auger maps using the OKVV and the Zr emissions show surface regions where only the Zr Auger lines are detected, whereas on pure ZrO2 powder this effect is not observed. Since it is possible to rule out from the XPS Zr3d core line spectra, the presence of metallic zirconium hydrogen spillover mechanisms is invoked to explain this result.

Microraman and scanning electron microscopy studies have been performed on pure TiO2 and Nb-Ti-O nanopowders obtained by laser induced synthesis. The effect of Nb content on the temperature of the anatase to rutile phase transformation, induced by annealing in air at different temperatures, has been evidenced and related to the changes in the particle size distributions obtained from a Fourier analysis of the X-ray diffraction patterns.

A new approach based on the study of distortion in the AO3 layer of ABO3 perovskites is proposed with the aim to discuss their ferroelectric properties. Rhombohedral distortions exist for either A-O average distances shorter than 2.7 A (space group Nr.161) or A-O distances larger than 3 Å (space group Nr.160). In the case of small distortions tetragonal or orthorhombic symmetries are preferred. Moreover, a relationship between the dimension of the B cation and the distortion in this type of structure has been established. Preliminary results show interesting correlations between distortions in the AO3 plane and the critical temperature of ferroelectric materials.

Structural studies have been carried out on SnO2 multilayer thin film grown by the Rheotaxial Growth and Thermal Oxidation method on A120 3 substrates. A preliminary analysis of the X-ray diffraction patterns shows that, in addition to the Sn0 2 cassiterite phase, a strong contribution from an orthorhombic Sn02 phase is present.

In the case of the 3-layer film, the orthorhombic phase is structurally and microstructurally stable after an annealing up to 32 h at 400 'C. The cation coordination is similar to that found in cassiterite, but the chains of edge-sharing [SnO6]8- octahedra run in a zig-zag fashion along the [100] direction, each straight unit containing four octahedra. The relationship between the two phases is discussed on the basis of structural simulations including twinning planes in the crystal structure.

In the present contribution an X-ray diffraction (XRD) study of thin films in the Mo-Bi-O system is reported. The samples were grown by MOCVD on A12O3 substrates. Several thin films have been grown starting from a Mo:Bi ratio in the two metallorganic precursors ranging from 6:1 to 1:1, thus obtaining films constituted by MoO3 and Mo-Bi-O layers with different thicknesses. The effect of the underlying Mo-Bi-O layer on the preferred orientation of the MoO3 layer, which is found in the samples with a high Mo:Bi ratio in the precursors, is discussed. Moreover, an equation is proposed relating the percentage of the phase constituting the film, as given by the Rietveld leastsquares procedure, and the film thickness. Thus it is shown that the growth rate of the pure MoO3 film is much higher than that of the Mo-Bi-O oxide film. A tentative explanation can be given by considering a possible growth inhibiting action by Bi in this system.

Based on X-ray diffraction and infrared spectroscopy measurements, BN thin films grown by PECVD on silicon substrates have been studied with the aim of identifying the thin film phase. In a set of samples, while the infrared spectra showed characteristic bands of the hexagonal phase, X - ray diffraction patterns only displayed reflections belonging to the cubic BN phase. Therefore, structural models have been developed to explain the apparent inconsistency between the two sets of experimental data. In particular, static disorder effects - which have been introduced in the model starting from the sp2 hybridization of the ordered hexagonal phase, as suggested by the infra-red spectroscopy results - allowed a consistent interpretation of the X-ray diffraction patterns. For another set of samples, which also showed a characteristic hexagonal signal in the IR data, the XRD pattern could not be indexed with any of the BN phases. In this case, the presence of molecular and ionic phases, associated with impurities, was considered in structural modeling studies.

We have investigated the conformation – order relationships of four aromatic polyimides prepared by thermal imidization of the precursor poly(amic acids) in thin films. They are: (i) PMDA-4,4′-ODA polyimide from pyromellitic dianhydride (PMDA) and 4,4′-oxydianiline (ODA) monomers; (ii) PMDA-PDA polyimide from PMDA and p-phenylene diamine (PDA); (iii) PMDA-Benzidine polyimide from PMDA and benzidine and (iv) BPDA-PDA polyirnide from biphenylene tetracarboxylicdianhydride (BPDA) and PDA. X-ray diffraction results and their analyses by molecular modeling show that all the four polyimides exhibit extended chain conformations in various smectic-type ordered structures that form monomer repeat layers but differ in the details of interchain packing. Furthermore, the polyimide chains are highly aligned along the film plane.