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Μελέτη με μετρήσεις ανακλαστικότητας ακτίνων-Χ προσρόφησης μορίων μικρού σχετικά μήκους (~ 2 nm) εντός πορώδους υμενίου αλουμίνας. Σκοπός της εργασίας είναι να διερευνηθεί καταρχήν η δυνατότητα της τεχνικής της ανακλαστικότητας να δώσει πληροφορίες για πορώδη υμένια, υμένια δηλαδή που η επιφάνειά τους παρουσιάζει μεγάλη τραχύτητα και κατόπιν να μελετηθεί η διείσδυση εντός των πόρων μορίων μικρού σχετικά μήκους. / Study with measurements of X-ray reflectivity, small molecules adsorption on length (~ 2 nm) in porous alumina film. The purpose of this paper is to explore the possibility of the reflectivity technique to provide information for porous films, films that the surface roughness is highly and then studied the penetration of molecules within the resources of a relatively small length.

Title: Microstructure and properties of multiferroic complex oxide thin films prepared by pulsed laser deposition method Author: Petr Machovec Department: Department of Condensed Matter Physics Supervisor: RNDr. Milan Dopita, Ph.D., Department of Condensed Matter Physics Abstract: In the frame of this thesis, structure, microstructure, and real structure of multiferroic epitaxial layers of LuFeO3 were studied by means of X-ray reflectivity and X-ray diffraction. In theoretical part the theory of X-ray scattering on crystalline layers is described. Standard description of X-ray reflectivity on series of rough layers is presented. Moreover, a model of X-ray scattering on mosaic layer is described. For experimental part of the work three samples were prepared by pulsed laser deposition method. First sample on sapphire substrate (Al2O3), second on platinum layer deposited on sapphire substrate and third on yttrium stabilized zirconia substrate. From the X-ray reflectivity curves the parameters such as layer thickness, interface roughness, surface roughness and material density, were determined. By analysing measured reciprocal space maps, lattice parameters and mosaic model parameters, such as mean mosaic block size, mosaic block size distribution, mosaic block misorientation and residual microstrain, were...

Surface and grain boundary electron scattering contribute significantly to resistivity as the dimensions of polycrystalline metallic conductors are reduced to, and below, the electron mean free path. A quantitative measurement of the relative contributions of surface and grain boundary scattering to resistivity is very challenging, requiring not only the preparation of suitably small conductors having independent variation of the two relevant length scales, namely, the sample critical dimension and the grain size, but also independent experimental quantification of these two length scales. In most work to date the sample grain size has been either assumed equal to conductor dimension or measured for only a small number of grains. Thus, the quantification of the classical size effect still suffers from an uncertainty in the relative contributions of surface and grain boundary scattering. In this work, a quantitative analysis of both surface and grain boundary scattering in Cu thin films with independent variation of film thickness (27 nm to 158 nm) and grain size (35 nm to 425 nm) in samples prepared by sub-ambient temperature film deposition followed by annealing is reported. Film resistivities of carefully characterized samples were measured at both room temperature and at 4.2 K and were compared with several scattering models that include the effects of surface and grain boundary scattering. Grain boundary scattering is found to provide the strongest contribution to the resistivity increase. However, a weaker, but significant, role is also observed for surface scattering. Several of the published models for grain boundary and surface scattering are explored and the Matthiessen's rule combination of the Mayadas and Shatzkes' model of grain boundary scattering and Fuchs and Sondheimer's model of surface scattering resistivity contributions is found to be most appropriate. It is found that the experimental data are best described by a grain boundary reflection coefficient of 0.43 and a surface specularity coefficient of 0.52. This analysis finds a significantly lower contribution from surface scattering than has been reported in previous works, which is in part due to the careful quantitative microstructural characterization of samples performed. The data does suggest that there is a roughness dependence to the surface scattering, but this was not conclusively demonstrated. Voids and impurities were found to have negligible impact on the measured resistivities of the carefully prepared films.

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Interfacial features of polymers are a complex, fascinating topic, and industrially very important. There is clearly a need to understand interactions between polymer layers as they can be used for controlling surface properties, colloidal stability and lubrication. The aim of my Ph.D study was to investigate fundamental phenomena of polymers at interfaces, covering adsorption, interactions between polymer layers and surfactants, surface forces and friction between adsorbed layers. A branched brush layer with high water content was formed on silica surfaces by a diblock copolymer, (METAC)m-b-(PEO45MEMA)n, via physisorption. The adsorption properties were determined using several complementary methods. Interactions between pre-adsorbed branched brush layers and the anionic surfactant SDS were investigated as well. Surface forces and friction between polymer layers in aqueous media were investigated by employing the Atomic Force Microscopy (AFM) colloidal probe technique. Friction forces between the surfaces coated by (METAC)m-b-(PEO45MEMA)n in water are characterized by a low friction coefficient. Further, the layers remain intact under high load and shear, and no destruction of the layer was noted even under the highest pressure employed, about 50 MPa. Interactions between polymer layers formed by a temperature responsive diblock copolymer, PIPOZ60-b-PAMPTMA17 (phase transition temperature of 46.1 °C), was investigated in the temperature interval 25-50 °C by using the AFM colloidal probe technique. Friction between the layers increases with increasing temperature (25-45 °C), while at 50 °C friction was found to be slightly lower than that at 45 °C. We suggest that this is due to decreased energy dissipation caused by PIPOZ chains crystallizing in water above the phase transition temperature. The structure of 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC) bilayers was determined by X-ray reflectometry. Surface forces and friction between DPPC bilayer-coated silica surfaces were measured utilizing the AFM colloidal probe technique. Our study showed that DPPC bilayers are able to provide low friction forces both in the gel (below ≈ 41°C) and in the liquid crystalline state (above ≈ 41°C). However, the load bearing capacity is lower in the gel state. This is attributed to a higher rigidity and lower self-healing capacity of the DPPC bilayer in the gel state. Friction forces in single asperity contact acting between a micro-patterned silicon surface and an AFM tip was measured in air. We found that both nanoscale surface heterogeneities and the µm-sized depressions affect friction forces, and considerable reproducible variations were found along a particular scan line. Nevertheless, Amontons’ first rule described average friction forces reasonably well. Amontons’ third rule and Euler’s rule were found to be less applicable to our system. / <p>QC 20141209</p>

In the UK, large quantities of intermediate level waste pose complex radiological remediation challenges. Chemical understanding of uranium in these Mg-rich sludges is vital. Previous studies have examined uranium uptake by calcium carbonate minerals (calcite and aragonite) under conditions pertinent to both natural and anthropogenically perturbed systems. However, research on uranyl uptake by magnesium-rich minerals such as magnesite [MgCO3], brucite [Mg(OH)2], nesquehonite [MgCO3·3H2O] and hydromagnesite-[Mg5(CO3)4(OH)2·4H2O] has not, to the best of our knowledge, been previously conducted. Such experiments will improve our understanding of the mobility of uranium and other actinides in natural lithologies such as dolomitic limestones or mafic igneous emplacements, as well as provide key information applicable to nuclear waste repository strategies involving Mg-rich phases. By two EXAFS techniques, we determined: (1) where uranyl (UO22+) is adsorbed, and (2) how uranyl is attached to the mineral surface. Therefore powder experiments of U(VI) were performed with magnesite, brucite, nesquehonite and hydromagnesite. The second experiment (GIXAFS) consisted of single crystals of magnesite (10.4) and brucite (0001). The powders were reacted in solution pH ~8.5 with U(VI)nitrate for 48 hrs. under ambient PCO2 = -3.5. The single crystals were reacted under ambient and reduced PCO2 ~ -4.5 for 48 hrs. with concentrations of U(VI)chlroride above (500; 50 ppm) and below (5 ppm) solubility of schoepite [UO2(OH)2·H2O]. The GIXAFS measurements were made at χ = 0˚ and χ = 90˚ relative to the synchrotron beam polarisation to uequivocally determine the adsorbate structures. Kd values for Mg-carbonate phases were comparable to or exceeded those published for calcium carbonates. GIXAFS results clearly showed polarisation for both ambient and reduced PCO2. XANES results showed uranyl is oriented with the axial oxygens perpendicular to the mineral surface. This implies, using also X-ray reflectivity and diffuse scatter, local hydrated bayleyite [Mg2(UO2)(CO3)3∙18H2O] and possible rutherfordine-like [UO2CO3] regions, which will be useful to predict uranium behaviour in various remediation processes.

The interfacial structuring of three non-halogenated ionic liquids was examined at the air-liquid interface for both dry and humid condition by analysis of X-ray reflectometry data using a slab model approach. The aim was to investigate the effect of humidity on the air-liquid interface. Pure ionic liquids as well as solutions of 5% w/w and 20% w/w in propylene carbonate were examined. Three different cations were used, a phosphonium cation ([P6,6,6,14]+) and two dialkylimidazolium cations ([C6C1Im]+ and [C10C1Im]+). The anion was bis(mandelato)borate ([BMB]-), which is a non-commercial anion that has been shown to exhibit excellent tribological properties. The results reveal that the presence of ambient water has an impact on the interfacial structure and the layering of all pure ionic liquids, as well as most cases of ionic liquid solutions. Exposure to humidity had the largest response in the case of all pure and diluted solutions of [C6C1Im][BMB], for which a more pronounced layering was observed. The [P6,6,6,14][BMB] solutions did not exhibit any significant changes when exposed to ambient water, with the 20% w/w solution proving to be the most stable. / Gränsskiktsstrukturen hos tre olika icke-halogenerade jonvätskor undersöktes vid luft-vätskegränsskiktet för både torra och fuktiga förhållanden genom analys av data från en röntgen reflektometer med en “slab model approach”. Målet var att undersöka effekten av luftfuktighet på luft-vätskagränsskiktet. Rena jonvätskor såväl som lösningar av 5 och 20 vikt-% utspädda i propylenkarbonat undersöktes. Tre olika katjoner användes, en fosforkatjon ([P6,6,6,14]+) samt två dialkylimidazoliumkatjoner ([C6C1Im]+ och [C10C1Im]+). Anjonen var bis(madelato)borat ([BMB]-), vilket är en icke-kommersiell anjon som har visat bra tribologiska egenskaper. Resultatet visar att närvaron av omgivande vatten har en påverkan på gränsskiktsstrukturen samt skiktning hos alla rena jonvätskor och de flesta utspädda lösningar. Exponering för fuktighet hade den största inverkan på alla rena och utspädda lösningar av [C6C1Im][BMB], för vilka en mer distinkt skiktning kunde observeras. [P6,6,6,14][BMB] lösningar uppvisade inga signifikanta ändringar vid exponering till fuktig luft, där den lösning med 20 vikt-% visade sig vara mest stabil.