The present thesis deals with optimization of the formation of thin layers of metallic materials. In the theoretical part was elaborated overview of the implementation of the formation of thin- film structures, particularly using vacuum techniques. Chemical and physical vapor deposition. They were described methods of pretreatment of thin layers. The findings were discussed methods of controlling the pre-treated surface, quality control and mutual adhesion of coating layers. In the experimental part of the pre-treatment methods were selected and applied to selected substrates. Pretreatments were evaluated using a control surface by wetting angles and by atomic force microscopy. Then, the metal structure formed of copper on the pretreated substrates. Implementation by means of magnetron sputtering. Adhesion layers was checked by testing the surface lattice method. The quality was observed by scanning electron microscopy. The results were used to design the technological process of making metal layers.

This diploma thesis deals with the design of composition and the study of properties of the ternary binding system based on purposeful ettringite formation, which was subsequently used for the preparation of self-leveling floor materials, specifically self-levelling underlay and thin-layer floor screed. In the designed compositions of the mixtures is then focused attention on optimizing the dosage of two kinds of plasticizer agents, followed by assessing their impact on the technological properties of these materials.

The work deals with the deposition of layers for electrochromic device with different methods. Transparent electrically conductive layer of SnO2 was deposited by pyrolytic decomposition of peroxostannate solution. Hydrogen peroxide in starting solution contributes to the oxidation process of growth layers and to increase the electrical conductivity. Active electrochromic layer of WO3 was electrolytic deposited from the peroxotungstic acid solution. Optimal deposition time and the optimal annealing temperature of deposited layers were found. Passive electrochromic layer of V2O5 was deposited using dip-coating method from peroxovanadate solution. A contribution of solution diluted with distilled water was investigated. Found results were used to construct complete electrochromic device with polymer gel electrolyte.

This master´s thesis is focused on measurement of optical properties of thin layer of materials used in organic solar cells (OSC). The usage of graphene oxides and its reduced forms as parts of hole transport layer (HLT) in OSC were studied. At the beginning of the thesis, there is described basic theory necessary to understand the optical properties of thin layers. The thin layer deposition and reduction of GO are discussed too. The experimental part is aimed to the optical characterization of prepared thin films. The results from optical microscopy, UV-VIS spectroscopy, FT-IR spectroscopy and spectroscopic ellipsometry were obtained. At the end of the thesis, the results are concluded and compared with already published literature.

In dieser Arbeit werden kalt-abgeschiedene Mehrkomponentenschichtelektroden hin-sichtlich ihrer elektrokatalytischen Eigenschaften untersucht. Die Mehrkomponenten-schichten aus Gold, Nickel und ggf. Antimon werden auf einem Kohlenstoffträgermaterial abgeschieden. Dabei handelt es sich um Metallkomponenten, die sich unter ther-modynamischen Bedingungen nicht mischen. Unter UHV-Bedingungen wird ein hochdispergierter bzw. amorpher Zustand erzwungen. Die frisch hergestellte Mehrkomponentenschicht ist elektrochemisch inert. Zyklovoltammetrische Untersuchungen führen zu dem Schluß, daß sich die Oberflächenschicht im elektrochemischen Experiment verändert. Die Elektrooxidation der Alkohole Methanol, Ethanol und Ethylenglykol in KOH-Lösung tritt erst nach einer Aktivierungsphase auf. Die elektrokatalytischen Eigenschaften der reinen Metalle treten zutage. Mittels der in situ Infrarotspektroskopie werden Formiat, Acetat und Glykolat als Oxidationsprodukte der obengenannten Alkohole identifiziert. Oberflächen-Ramanmessungen werden unter der Fragestellung durchgeführt, ob die kalt-abgeschiedenen Schichten einen Oberflächenverstärkungseffekt (SERS-Effekt) zeigen: Es werden Ramanmessungen von Pyridin als Sondenmolekül in KOH-Lösung an Mehrkomponentenschichtelektroden und an massiven Mehrkomponentenelektroden durchgeführt. / The electrooxidation of methanol, ethanol and ethylene glycol at cold deposited trimetallic thin layers of gold, nickel and antimony on glassy carbon in contact with an alkaline electrolyte solution was studied with cyclic voltammetry and in situ infrared reflection absorption spectroscopy. A new procedure of spectra acquisition resulting in an improved suppression of spurious bands caused by volatile components in the sample chamber of the infrared spectrometer was employed. Formate, acetate and glycolate are detected as oxidation products. The thin layer electrodes are also investigated with Raman spectroscopy (surface enhanced Raman spectroscopy), whereby pyridine is used as probe molecule.

(EN) In the first part of this work, analytical methods for determination of impurities of active pharmaceutical ingredients (API) in combined pharmaceutical dosage forms were developed and validated. Development of the methods covered both the optimization of sample preparation procedure and chromatographic conditions. The methods were validated according to International Conference on Harmonization guideline and both of them were confirmed to be able to analyze stability samples. Impurities in paracetamol, codeine phosphate hemihydrate and pitophenone hydrochloride in the presence of fourth API fenpiverinium bromide were separated by using ion-pair reversed phase chromatography with gradient elution. Symmetry C18, 250 x 4,6 mm, 5 µm heated to 35 řC was used as a separation column. A diode array detector was used. The detection wavelengths were set as follows: 220 nm for paracetamol impurity K, 245 nm for paracetamol and its other impurities and 285 nm for codeine, pitophenone and their impurities. Impurities in valsartan, amlodipine besylate and hydrochlorothiazide were separated by reversed phase UHPLC method with gradient elution. Chromatographic column Zorbax Eclipse C8 RRHD, 100 x 3,0 mm, 1,8 µm heated to 30 řC and spectrophotometric detection were used. The detection wavelengths were set as...

Railway tracks experience elevated rail deflections when the supporting soil is soft and/or the train speed is greater than approximately 50% of the wave propagation velocity in the track-soil system (i.e. the critical velocity). Such vibrations are undesirable, so soil replacement or soil improvement of the natural soil (or alternatively mini-piles or lime-cement treatment) is often used to increase track-ground stiffness prior to line construction. Although areas of existing soft subgrade might be easily identified on a potential new rail route, it is challenging to determine the type and depth of ground remediation required. Therefore, major cost savings can be made by optimising ground replacement/improvement strategies. This paper presents a numerical railway model, designed for the dynamic analysis of track-ground vibrations induced by high speed rail lines. The model simulates the ground using a thin-layer finite element formulation capable of calculating 3D stresses and strains within the soil during train vehicle passage. The railroad track is modelled using a multi-layered formulation which permits wave propagation in the longitudinal direction, and is coupled with the soil model in the frequency-wavenumber domain. The model is validated using a combination of experimental railway field data, published numerical data and a commercial finite element package. It is shown to predict track and ground behaviour accurately for a range of train speeds. The railway simulation model is computationally efficient and able to quickly assess dynamic, multi-layered soil response in the presence of ballast and slab track structures. Therefore it is well-suited to analysing the effect of different soil replacement strategies on dynamic track behaviour, which is particularly important when close to critical speed. To show this, three soil-embankment examples are used to compare the effect of different combinations of stiffness improvement (stiffness magnitude and remediation depths up to 5 m) on track behaviour. It is found that improvement strategies must be carefully chosen depending upon the track type and existing subgrade layering configuration. Under certain circumstances, soil improvement can have a negligible effect, or possibly even result in elevated track vibration, which may increase long-term settlement. However, large benefits are possible, and if detailed analysis is performed, it is possible to minimise soil improvement depth with respect to construction cost.

<p>Sukcinimidi su jedinjenja koja pokazuju vi&scaron;estruke farmakolo&scaron;ke efekte uključujući i antiproliferativnu aktivnost, zahvaljujući prisustvu farmakofore sa dva hidrofobna regiona i dva regiona bogata elektronima. Savremeni dizajn lekova ima za cilj da se modifikacijama u strukturi (promena vrste, položaja i orijentacije supstituenata) i in silico računarskim metodama predvide i optimizuju farmakokinetske osobine i bezbednosni profil kandidata za lek. U ranoj fazi razvoja lekova se koriste postojeće baze podataka o molekulskim, farmakokinetskim i toksikolo&scaron;kim parametrima već ispitanih jedinjenja i pomoću matematičkih modela i algoritama predviđaju se osobine novih molekula, elimini&scaron;u se neodgovarajući kandidati i postiže se u&scaron;teda u vremenu i materijalnim sredstvima. Da se ispitaju fizičko-hemijske karakteristike 11 novosintetisanih metil-etil-N-aril-sukcinimida na osnovu strukture, primenom različitih softverskih paketa; da se na osnovu strukture odrede farmakokinetski i toksikolo&scaron;ki parametri, primenom različitih softverskih paketa; da se ispita retenciono pona&scaron;anje, odnosno odrede retencione konstante za svako jedinjenje primenom visokoefikasne hromatografije na tankom sloju (HP-TLC) i ispita mogućnost primene retencionih konstanti kao mere lipofilnosti ispitivanih jedinjenja; da se ispita antiproliferativna aktivnost na odabranim kulturama ćelija karcinoma i na zdravim ćelijama fibroblasta pluća; da se analizom molekulskog dokinga ustanovi vezivanje za estrogene receptore. Ispitano je retenciono pona&scaron;anje 11 novosintetisanih derivata sukcinimida primenom visokoefikasne hromatografije na tankom sloju (HP-TLC) obrnute faze uz primenu dvokomponentne sme&scaron;e vode i organskog rastvarača (metanola, acetonitrila ili acetona), sa odgovarajućim zapreminskim udelom organskog rastvarača kao mobilne faze. Iz razvijenih hromatograma su izračunate retencione konstante RM0 i S. Logaritam podeonog koeficijenta (logP) određen je in silico, kori&scaron;ćenjem različitih računarskih programa. In silico su određene fizičko-hemijske karakteristike, farmakokinetski parametri, toksikolo&scaron;ki parametri, akvatična toksičnosti i afinitet vezivanja za estrogene receptore. Izračunate su vrednosti afiniteta za 4 vrste receptora (G-protein spregnuti receptori, jonski kanali, inhibitori kinaza, nuklearni receptori). Antiproliferativna aktivnost ispitivanih derivata sukcinimida određena je primenom kolorimetrijskog testa sa tetrazolijum solima (MTT testa) na komercijalnim kulturama ćelija (MRC-5, A549, HeLa, MDA-MB-231, MCF-7, HT-29) i izračunate su IC50 vrednosti. Urađena je i doking analiza sukcinimida prema ERA (estrogen receptor alfa) i ERB (estrogen receptor beta) i dobijene su vrednosti energije formiranja kompleksa sa posmatranim receptorima (MolDock Score). Statistički najznačajnije linearne korelacije dobijene su između eksperimentalno određenih hromatografskih parametara (RM0 i S) i in silico parametara lipofilnosti MlogP i ClogP. Ispitivanjem uticaja promene RM0 i S na farmakokinetske karakteristike dobijeni su rezultati koji pokazuju paraboličnu zavisnost konstante apsorpcije (Ka) i procenta vezivanja za proteine plazme (PPB) od posmatranih retencionih konstanti, dok je zavisnost sa volumenom distribucije (Vd) i sposobno&scaron;ću prolaska kroz krvno-moždanu barijeru (logBBB) bila linearnog tipa. Toksičnost ispitivanih jedinjenja, procenjena na osnovu in silico dobijenih LD50 vrednosti, nije bila vi&scaron;a od toksičnosti već registrovanih lekova sa strukturom sukcinimida, i dala je parabolične zavisnosti u odnosu na RM0 i S vrednosti. Eksperimentalno nijedno od ispitivanih jedinjenja nije pokazalo aktivnost u odnosu na zdrave fibroblaste pluća. Najznačajniju antiproliferativnu aktivnost (najniže IC50) su pokazala jedinjenja 6 i 7 u odnosu na ćelije linije MCF-7 i jedinjenje 11 u odnosu na A549 ćelijsku liniju. Doking analiza je pokazala niže energije formiranja kompleksa sa ERA, u odnosu na ERB. Eksperimentalno određeni parametri RM0 i S se mogu koristiti kao alternativne i pouzdane mere lipofilnosti analiziranih sukcinimida. Ispitivana jedinjenja pokazuju povoljne fizičko-hemijske karakteristike, predviđene in silico metodama i povoljne farmakokinetske karakteristike: male vrednosti konstante apsorpcije, umeren volumen distribucije, povoljan afinitet vezivanja za proteine plazme, favorizovan prolazak kroz krvno-moždanu barijeru za lipofilnija jedinjenja. Procenjuje se da sva ispitivana jedinjenja, izuzev derivata sa &ndash;CN supstituentom, imaju zahtevani nizak stepen toksičnosti. Po antiproliferativnoj aktivnosti u odnosu na ćelije ER-zavisnog karcinoma dojke (MCF-7) izdvajaju se jedinjenja sa metil i nitro supstituentom u para položaju. Na osnovu malih energija formiranja kompleksa sa ERA, koji su eksprimirani na ćelijama MCF-7 linije, pretpostavlja se da bi mehanizam njihovog delovanja delimično mogao biti obja&scaron;njen uticajem na ERA, ali su potrebna dodatna istraživanja na tom polju.</p> / <p>Succinimides have exhibited various pharmaceutical effects including antiproliferative activity due to an important structural fragment (a pharmacophore) presented in form of two hydrophobic regions and two electron-rich centers. Current development of new drugs involves modifications in structure (type, position and orientation of substituents) and usage of in silico computational programs to predict and optimize pharmacokinetic and safety profile of drug candidates. In early phase of drug development, databases regarding the molecular, pharmacokinetic and toxicological parameters of already tested compounds are used, mathematical models and algorithms are applied for predicting the properties of new molecules and inadequate candidates are eliminated saving time and resources. Determination of physico-chemical properties of the analyzed methyl-ethyl-N-phenilsuccinimide derivatives by software packages; virtual pharmacokinetic and toxicology screening; investigation of retention behavior of the compounds by the reversed-phase HPTLC analysis and calculation of retention constants and their correlation with lipophilicity; in vitro evaluation of antiproliferative activity toward five carcinoma cell lines and normal fetal lung cell line; molecular behavior study on target estrogen receptors by molecular docking and correlation of antiproliferative activity toward ER+ breast carcinoma cell lines and in silico estrogen receptor affinity binding. Retention behavior of 11 newly synthesized succinimide derivatives was determined by reversed phase high performance thin layer chromatography (RP HPTLC) with the application of two-component mixtures water - organic solvent (methanol, acetonitrile or acetone) with adequate volume fractions of the organic modifier. After chromatographic development RM0 and S parameters were calculated. The logarithm of partition coefficient, logP for the analyzed compounds were calculated by different softwares. Physico-chemical properties, pharmacokinetic and toxicological parameters, aquatic toxicity and relative affinity to estrogen receptors were predicted in silico. The affinity toward 4 types of receptors (G-proteine coupled receptors, ion channels, kinase inhibitors, nuclear receptors) were calculated as well. Standard MTT assay was applied to evaluate cytotoxic activities of the analyzed succinimides after cells were exposed. Antiproliferative activity were investigated toward commercial MRC-5, A549, HeLa, MDA-MB-231, MCF-7, HT-29 cell lines and IC50 values were calculated for each compound. MolDock Score that represents energy of binding to estrogen alfa and estrogen beta receptors was determined by molecular docking. Statistically significant linear correlations were determined between the chromatographic retention constants (RM0 and S) and calculated logP, and the best two were obtained in correlation of retention constants with MlogP and ClogP. The examination of RM0 and S influence on pharmacokinetics indicated parabolic dependence of the absorption constant (Ka) and plasma protein binding predictor (PPB) from the observed constants while the volume of distribution (Vd) and the ability to cross the brain blood barrier (logBBB) had linear association with the retention parameters. The toxicity of the analysed compounds evaluated in silico as LD50 on rodents was lower in comparison with the drugs with succinimide structure that are on the market and had parabolic correlation with the RM0 and S values. The experiments indicated that none of the compounds examined had cytotoxic activity toward the healthy lung fibroblast cells. The results of the in vitro assay shown that none of the investigated compounds demonstrated antiproliferative activity toward fetal lung cells. The most potent antiproliferative agents were compounds 6 and 7 toward MCF-7 cell line, and compound 11 toward A549 cell line. Molecular docking shown lower energy for binding to ERA in comparison to ERB.</p>

We study the question of periodic homogenization of a variably scaled reaction-diffusion equation with non-linear drift of polynomial type. The non-linear drift was derived as hydrodynamic limit of a totally asymmetric simple exclusion process (TASEP) for a population of interacting particles crossing a domain with obstacle. We consider three different geometries: (i) Bounded domain crossed by a finitely thin flat composite layer; (ii) Bounded domain crossed by an infinitely thin flat composite layer; (iii) Unbounded composite domain.\end{itemize} For the thin layer cases, we consider our reaction-diffusion problem endowed with slow or moderate drift. Using energy-type estimates as well as concepts like thin-layer convergence and two-scale convergence, we derive homogenized evolution equations and the corresponding effective model parameters. Special attention is paid to the derivation of the effective transmission conditions across the separating limit interfaces. As a special scaling, the problem with large drift is treated separately for an unbounded composite domain. Because of the imposed large drift, this nonlinearity is expected to explode in the limit of a vanishing scaling parameter. To deal with this special case, we employ two-scale formal homogenization asymptotics with drift to derive the corresponding upscaled model equations as well as the structure of the effective transport tensors. Finally, we use Schauder's fixed point Theorem as well as monotonicity arguments to study the weak solvability of the upscaled model posed in the unbounded domain. This study wants to contribute with theoretical understanding needed when designing thin composite materials which are resistant to slow, moderate, and high velocity impacts. / We study the question of periodic homogenization of a variably scaled reaction-diffusion equation with non-linear drift of polynomial type. The non-linear drift was derived as hydrodynamic limit of a totally asymmetric simple exclusion process (TASEP) for a population of interacting particles crossing a domain with obstacle. We consider three different geometries: (i) Bounded domain crossed by a finitely thin composite layer; (ii) Bounded domain crossed by an infinitely thin composite  layer; (iii) Unbounded composite domain. For the thin layer cases, we consider our reaction-diffusion problem endowed with slow or moderate drift. Using energy-type  estimates, concepts like thin-layer convergence and two-scale convergence, we derive  homogenized  equations. Special attention is paid to the derivation of the effective transmission conditions across the separating limit interfaces. The problem with large drift is treated separately for an unbounded composite domain. Because of the imposed large drift, this nonlinearity is expected to explode in the limit of a vanishing scaling parameter.  This study wants to contribute with theoretical understanding needed when designing thin composite materials which are resistant to slow, moderate, and high velocity impacts.

Au vu des limitations rencontrées par la miniaturisation des circuits microélectroniques, l’augmentation de performances des systèmes repose largement aujourd’hui sur la fabrication d’empilements de couches minces complexes et innovants pour offrir davantage de compacité et de flexibilité. L’intérêt grandissant pour la réalisation de structures innovantes temporaires, i.e. permettant de réaliser des circuits sur les deux faces d’un même film, nous a mené à évaluer les potentialités d’une technologie combinant le transfert de films minces monocristallins, i.e. la technologie Smart Cut™, et un procédé de de porosification partielle du silicium afin de mettre au point une technologie de double report de film monocristallin. En ce sens, des substrats de silicium monocristallin ont été partiellement porosifiés par anodisation électrochimique. La mise en œuvre de traitements de substrats partiellement poreux a nécessité l’emploi de techniques de caractérisation variées pour dresser une fiche d’identité des couches minces poreuses après anodisation et évaluer l’évolution des propriétés de ces couches en fonction des différents traitements appliqués. Les propriétés chimiques, structurales et mécaniques des couches de Si poreux ont ainsi été étudiées via l’utilisation de différentes techniques de caractérisation (XPS-SIMS, AFM-MEB-XRD, nanoindentation, technique d’insertion de lame, etc.). Ces études ont permis d’appréhender et de décrire les mécanismes physiques mis au jeu au cours des différents traitements et de déterminer les caractéristiques {porosité, épaisseur} optimales des couches poreuses compatibles avec les séquences de la technologie proposée. La technologie Smart Cut™ a ainsi été appliquée à des substrats partiellement porosifiés menant à la fabrication réussie d’une structure temporaire de type Silicium-sur-Isolant avec une couche de silicium poreux enterrée. Ces structures temporaires ont été « démontées » dans un second temps par collage polymère ou collage direct et insertion de lame menant au second report de film mince monocristallin par rupture au sein de la couche porosifiée et donc fragile. Les structures fabriquées ont été caractérisées pour vérifier leur intégrité et leurs stabilités chimique et mécanique. Les propriétés cristallines du film mince de Si monocristallin, reporté en deux temps, ont été vérifiées confirmant ainsi la compatibilité des structures fabriquées avec des applications microélectroniques telles que les applications de type « Back-Side Imager » nécessitant une implémentation de composants sur les deux faces du film. Ainsi une technologie prometteuse et performante a pu être élaborée permettant le double report de films minces monocristallins et à fort potentiel pour des applications variées comme les imageurs visibles ou le photovoltaïque. / As scaling of microelectronic devices is confronted from now to fundamental limits, improving microelectronic systems performances is largely based nowadays on complex and innovative stack realization to offer more compaction and flexibility to structures. Growing interest in the fabrication of innovative temporary structures, allowing for example double sided layer processing, lead us to investigate the capability to combine one technology of thin single crystalline layer transfer, i.e. the Smart Cut™ technology, and partial porosification of silicon substrate in order to develop an original double layer transfer technology of thin single crystalline silicon film. To this purpose, single crystalline silicon substrates were first partially porosified by electrochemical anodization. Application of suitable treatments of porous silicon layer has required the use of several characterization methods to identify intrinsic porous silicon properties after anodization and to verify their evolution as function of different applied treatments. Chemical, structural and mechanical properties of porous silicon layers were studied by using different characterization techniques (XPS-SIMS, AFM-MEB-XRD, nanoindentation, razor blade insertion, etc.). Such studies allowed comprehending and describing physical mechanisms occurring during each applied technological steps and well determining appropriated {porosity, thickness} parameters of porous silicon layer with the developed technological process flow. The Smart Cut™ technology was successfully applied to partially porosified silicon substrates leading to the fabrication of temporary SOI-like structures with a weak embedded porous Si layer. Such structures were then “dismantled” thanks to a second polymer or direct bonding and razor blade insertion to produce a mechanical rupture through the fragile embedded porous silicon layer and to get the second thin silicon film transfer. Each fabricated structure was characterized step by step to check its integrity and its chemical and mechanical stabilities. Crystalline properties of the double transferred silicon layer were verified demonstrating the compatibility of such structures with microelectronic applications such as “Back-Side Imagers” needing double-sided layer processing. Eventually, a promising and efficient technology has been developed to allow the double transfer of thin single crystalline silicon layer which presents a high potential for various applications such as visible imagers or photovoltaic systems.