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Total scattering can be used to study crystalline materials, whose structure presents a periodic arrangement of atoms, as well as disordered materials, such as liquids, glasses or nanomaterials. This thesis work reports three experimental case studies in which different analysis methods were chosen as appropriate on a case-by-case basis. This study demonstrates that total scattering combined with modelling and complementary experimental techniques can guide the understanding of the structure of complex nanostructures. X-ray and neutron total scattering data were collected on multi-walled carbon nanotubes continuously filled with iron and analysed using the program PDFgui for refinement of the pair distribution function and molecular dynamics simulations using the program DL_Poly_4. The analyses show that the iron core is mainly composed of ��-Fe and confirms the dependence of the local ordering on the orientation of the crystallographic axes of iron with respect to the nanowire axis. Prussian blue (Fe4[Fe(CN)6]3 · ��H2O) was synthesised in bulk and nanoparticulate phases using deuterated chemicals; the amount of D2O and H2O in the pores and vacancies, as well as polyvinylpyrrolidone remaining in the nanoparticle samples, were estimated, using an ad hoc modelling procedure of the first few peaks in the neutron PDF function. Models of the structure were refined using the programs PDFgui and RMCProfile. In the last case, a 50Å supercell of the bulk structure with randomly distributed stoichiometric vacancies and D2O and H2O molecules occupying both the pores and the vacancies was used as starting atomic configuration. The CaO/CaCO3 family of materials consists of a series of samples that have undergone carbonation and/or calcination. The X-ray and neutron pair distribution function data were compared to the theoretical PDF of the CaO and CaCO3 phase, generated using the program GULP, that produces PDF functions based on the spectrum of phonon frequencies of the material. The analysis shows that the carbonation is almost completed already after 2 minutes of carbonation and the structure remains stable under further carbonation.

Texture, i.e. preferred orientation, can cause large systematic errors in quantitative analysis of crystalline materials using x-ray powder diffraction (XRPD) data. Various mathematical forms have been proposed for the application of preferred orientation corrections. The most promising of these appears to be the single-parameter March (1932) model proposed by Dollase (1986).Li and O'Connor (1989) applied the March model to determine the level of preferred orientation in various gibbsites using two procedures. The first involved the Rietveld (1969) least squares pattern-fitting method. Each pattern was Rietveld-analysed in two ways, initially assuming random orientation of the crystallites and subsequently with the March model. The second procedure for preferred orientation analysis, described here as the line ratio method, determines preferred orientation factors according to the intensity ratios of carefully selected line pairs.In the thesis the procedures proposed by Li and O'Connor for texture analysis have been evaluated with XRPD data sets for molybdite, calcite and kaolinite. The results indicate that while the March formula improves agreement between the' calculated and measured patterns in Rietveld analysis, other forms of systematic error in the intensity data appear to limit the effectiveness of the March formula in general. It has been found also that the line ratio method improves agreement between the data sets, but less effectively than the Rietveld method. It is proposed that extinction is likely to be the most influential source of systematic error competing with texture.

Amorphous selenium based digital radiography has attracted much attention because of selenium's high X-ray absorption and excellent charge transport properties, and the ability to be created thick (typically 100 to 1000 micron) uniform layers over a large area (typically 30 cm X 30 cm) at low processing temperatures (typically at around 50 degree C substrate temperature). In this work, the excess noise in amorphous selenium has been studied. A number of device parameters were altered to study the noise characteristics, such as the metal of the electrodes, bulk material composition, device volume, surface conditions and substrate temperature. All the samples had a transverse geometry with 20 to 200- micron thick layers of amorphous selenium electroded with metal at the top and at the bottom. Sample devices were fabricated by conventional vacuum deposition.<p> Noise power was measured over a limited bandwidth of 1 kHz. The fluctuations for one sample amounted to 1% of the bias current. The excess noise was mainly 1/<i>f</i> noise with the slope ranging from -0.77 to -1.4. Interpretation of the noise spectra was complicated due to the samples' highly non-linear I-V relation and long time transients.<p> The metals of the electrode clearly showed a large effect on both the magnitude and shape of the noise spectrum. Of the metals studied, aluminum produced the least normalized noise and platinum the most. The addition of arsenic caused a decrease in the normalized noise. An additional 0.2% (% wt.) arsenic decreased the 1/<i>f</i> noise magnitude by more than a decade, but did not change the slope. The addition of chlorine did not affect the noise magnitude. Amorphous selenium is quite vulnerable to stress and in particular, external mechanical stress causes crystallization. The surface of the sample was gently abraded, applying the least possible amount of stress to the selenium layer. A change in the surface condition before the top electrode was deposited showed that a roughened surface decreased the noise magnitude substantially. These results strongly indicate that the noise is controlled by the metal-semiconductor interface.<p> Noise characteristics in multilayered samples were examined. The p-i-n and n-i-p structures consisted of 200 micron i-layer with 2 to 6 micron p- and n-like layers. The noise fluctuation in the current are typical of 1/<i>f</i> noise showing a power-law spectrum with slopes between -0.9 to -1.1. These samples showed a substantial decrease in the noise power compared to single layer samples; the additional n-like and p-like layers acted as carrier sources so that the current was not controlled by the metal interface. Hence, the measurements are closer to the intrinsic noise of a-Se. After exposure to 14 R (Roentgen) of X-rays, the normalized noise decreased by a factor of 1.6 for the n-i-p structure.

Amorphous selenium based digital radiography has attracted much attention because of selenium's high X-ray absorption and excellent charge transport properties, and the ability to be created thick (typically 100 to 1000 micron) uniform layers over a large area (typically 30 cm X 30 cm) at low processing temperatures (typically at around 50 degree C substrate temperature). In this work, the excess noise in amorphous selenium has been studied. A number of device parameters were altered to study the noise characteristics, such as the metal of the electrodes, bulk material composition, device volume, surface conditions and substrate temperature. All the samples had a transverse geometry with 20 to 200- micron thick layers of amorphous selenium electroded with metal at the top and at the bottom. Sample devices were fabricated by conventional vacuum deposition.<p> Noise power was measured over a limited bandwidth of 1 kHz. The fluctuations for one sample amounted to 1% of the bias current. The excess noise was mainly 1/<i>f</i> noise with the slope ranging from -0.77 to -1.4. Interpretation of the noise spectra was complicated due to the samples' highly non-linear I-V relation and long time transients.<p> The metals of the electrode clearly showed a large effect on both the magnitude and shape of the noise spectrum. Of the metals studied, aluminum produced the least normalized noise and platinum the most. The addition of arsenic caused a decrease in the normalized noise. An additional 0.2% (% wt.) arsenic decreased the 1/<i>f</i> noise magnitude by more than a decade, but did not change the slope. The addition of chlorine did not affect the noise magnitude. Amorphous selenium is quite vulnerable to stress and in particular, external mechanical stress causes crystallization. The surface of the sample was gently abraded, applying the least possible amount of stress to the selenium layer. A change in the surface condition before the top electrode was deposited showed that a roughened surface decreased the noise magnitude substantially. These results strongly indicate that the noise is controlled by the metal-semiconductor interface.<p> Noise characteristics in multilayered samples were examined. The p-i-n and n-i-p structures consisted of 200 micron i-layer with 2 to 6 micron p- and n-like layers. The noise fluctuation in the current are typical of 1/<i>f</i> noise showing a power-law spectrum with slopes between -0.9 to -1.1. These samples showed a substantial decrease in the noise power compared to single layer samples; the additional n-like and p-like layers acted as carrier sources so that the current was not controlled by the metal interface. Hence, the measurements are closer to the intrinsic noise of a-Se. After exposure to 14 R (Roentgen) of X-rays, the normalized noise decreased by a factor of 1.6 for the n-i-p structure.