In der vorliegenden Arbeit wird das Wachstum von Ta- und TaN-Schichten auf Si- und SiO_2-Substraten untersucht Die Schichten werden dabei unter technologienahen Bedingungen mittels Magnetron-Sputtern abgeschieden. Die Untersuchungen erfolgen hauptsächlich mit winkelaufgelöster röntgenstrahlungsangeregter Photoelektronenspektroskopie (ARXPS). Die Analysen erfolgen in situ, ohne Unterbrechung des Ultrahochvakuums, um die Deposite vor Oxidation und Kontamination zu schützen. Zur zerstörungsfreien Tiefenprofilanalyse wird ein Quantifizierungsalgoritmus beschrieben und angewandt. Für die Kombination Ta/Si wird die Bildung einer zunächst unvollständigen TaSi_2-Schicht, danach das Aufwachsen von Ta auf diese Zwischenschicht beobachtet. Für die Kombination Ta/SiO_2 wird eine Reduktion des SiO_2-Substrates bei gleichzeitigem Aufwachsen von Ta-Oxiden beobachtet. Auf dem durchmischten Schichtstapel wächst danach Ta auf. Für die Kombination TaN/Si wird die Bildung einer Si-N-Zwischenschicht bei gleichzeitigem Wachsen einer TaN-Schicht beobachtet. Für die Kombination TaN/SiO_2 wird das Aufwachsen einer TaN-Schicht ohne Ausbilung von Zwischenschichten beobachtet. Das Wachstumsverhalten des Ta/Si-Systems wird zusätzlich mit in situ Rastertunnelmikroskopie und -spektroskopie untersucht. Es wurden Untersuchungen zur thermischen Stabilität von abgeschiedenen Schichten an den Systemen Ta/Si und TaN/SiO_2 durchgeführt. Als mögliche Alternative zur winkelaufgelösten XPS wurden Untersuchungen mittels synchrotronstrahlungsangeregter Photoelektronenspektroskopie bei variierter Anregungsenergie durchgeführt.

Gegenstand der wissenschaftlichen Arbeit ist der technologische Nachweis für die Erzeugbarkeit haftfester metallischer und keramischer Schichten auf textilen Flächengebilden mit den PVD-Technologien reaktives Magnetron-Sputtern und reaktives Vakuumbogen-Verdampfen. Basis für die Realisierung der experimentellen Untersuchungen sind sowohl vorhandene industrielle PVD-Beschichtungsanlagen, die im Batchbetrieb arbeiten, als auch Rollcoater als Bindeglied zwischen einer Labor- und einer Industrieanlage. Kern des Vorhabens sind umfangreiche Batchbeschichtungen auf Basis einer breit angelegten Experimentalmatrix bezüglich Substrat- und Schichtauswahl. Gängige Targetmaterialien sind Kupfer, Aluminium und Silber. Um zu zeigen, dass über das thermische Bedampfen hinaus neue Schichten und Schichtsysteme auf textilen Faserstoffen abgeschieden werden können, wurden zusätzlich die Targetmaterialien Titan und Zirkonium in die Untersuchungen einbezogen. Zur Herstellung sowohl metallischer als auch keramischer Schichten wird neben den technologischen Parametern Beschichtungszeit und Schichtmaterial der Reaktivgasfluss variiert. Als Substrate kamen zwei leichtgewichtige PA 6.6-Gewebe mit unterschiedlicher Bindung, ein kalanderverfestigter Vliesstoff aus PES und ein Spinnvliesstoff aus Kern-Mantel-Fasern mit einem PA 6 Mantel zum Einsatz. Zur Verbesserung der Schichthaftungen wurden Versuche zur Vorbehandlung mittels Plasmabehandlung in Argon und Sauerstoff, mit Gasphasenfluorierung sowie HMDSO-Behandlung mit einem PA 6.6-Gewebe durchgeführt. Im Anschluss an die Vorbehandlung wurden die Proben mit Titan und Titannitrid metallisiert. Die Charakterisierung der Substrat-Schicht-Verbunde erfolgt hinsichtlich - der chemischen Zusammensetzungen der Schichten mittels ESCA (Electron Spectroscopy for Chemical Analysis), - der Schichtstrukturen und Fasermorphologien mittels Rasterelektronenmikroskopie, - der E-Moduln an Referenzprobekörpern aus Edelstahl mittels Härtemessung, - der Schichthaftungen durch Waschversuche, Martindale-Scheuertest, Peel-Test und - der funktionellen Schichteigenschaften wie Oberflächenwiderstände, elektromagnetische Schirmdämpfung, Wärmedämmeigenschaften Im Ergebnis der experimentellen Untersuchungen werden grundlegende Erkenntnisse zum Einfluss der PVD-Technologien und der Prozessparameter auf genannte Schicht- und Fasereigenschaften aufgezeigt. Des Weiteren werden die Zusammenhänge zwischen Schichtstruktur, Fasermorphologie und Schichthaftung dargelegt. Aus den Ergebnissen werden Schlussfolgerungen für eine gezielte industrielle Anwendung und Vorschläge für weiterführende wissenschaftliche Arbeiten abgeleitet. Die PVD-Verfahren werden bezüglich ihrer Eignung für die Textilbeschichtung bewertet. / Subject of the scientific study is the technological proof for the possibility to generate well adherent metallic and ceramic layers on textile fabrics with the PVD technologies reactive magnetron sputtering and reactive arc evaporation. Basis for the experimental investigations were both an industrial PVD coating device of the batch-type and a roll-coater which is a connective link between a laboratory and an industrial coating device. Extensive batch coatings on basis of a broadly applied experimental matrix in terms of the choice of the substrate and layer material are basis of the project. Usual target materials were copper, aluminium and silver. Additionally, the target materials titanium and zirconium were included in the investigations in order to show that new layers and layer systems can be deposited on textile fabrics by means of the investigated PVD technologies in comparison with thermal evaporation. Apart from the technological parameters coating time and layer material, the reactive gas flow were varied to deposit both metallic and ceramic layers. Substrates used in this study were lightweight Pa 6.6 fabrics with different weaves of the fabric, a calender bonded nonwoven of PES and a spunbonded nonwoven consisting of sheath-core fibers of PES (sheath) and Pa 6 (core). In order to improve the adhesion of layers, different pretreatments of the PA 66 fabric were carried out by means of plasma treatment with argon and oxygen, gas phase fluorination and treatment with HMDSO respectively. Subsequently, the pretreated samples were metallized with titanium and titanium nitride. The characterisation of the substrate layer combinations were carried out regarding - the chemical compositions of the layers by means of ESCA (Electron Spectroscopy for Chemical Analysis), - the layer structures and fiber morphologies by means of raster electron microscopy, - the modulus of elasticity on reference specimens consisting of stainless steel by means of hardness measurement, - the layer adhesion by wash tests, Martindale abrasion test, peel tests and - the functional layer characteristics such as surface resistances, electromagnetic shielding, heat insulating characteristics In the result of the experimental investigations, extensive knowledge to the influence of the PVD technologies and process parameters on layer and fiber characteristics are presented. Furthermore, the correlation of layer structure, fiber morphology and layer adhesion are explained. Conclusions for a selective industrial application and suggestions for further scientific investigations are derived from the results. The PVD procedures are evaluated concerning their suitability for the coating of textiles.

Vibration control requires high dynamic stiffness in mechanical structures for a reliable performance under extreme conditions. Dynamic stiffness composes the parameters of stiffness (K) and damping (η) that are usually in a trade-off relationship. This thesis study aims to break the trade-off relationship. After identifying the underlying mechanism of damping in composite materials and joint interfaces, this thesis studies the deposition technique and physical characteristics of nano-structured HDS (high dynamic stiffness) composite thick-layer coatings. The HDS composite were created by enlarging the internal grain boundary surface area through reduced grain size in nano scale (≤ 40 nm). The deposition process utilizes a PECVD (Plasma Enhanced Chemical Vapour Deposition) method combined with the HiPIMS (High Power Impulse Magnetron Sputtering) technology. The HDS composite exhibited significantly higher surface hardness and higher elastic modulus compared to Poly(methyl methacrylate) (PMMA), yet similar damping property. The HDS composites successfully realized vibration control of cutting tools while applied in their clamping interfaces. Compression preload at essential joint interfaces was found to play a major role in stability of cutting processes and a method was provided for characterizing joint interface properties directly on assembled structures. The detailed analysis of a build-up structure showed that the vibrational mode energy is shifted by varying the joint interface’s compression preload. In a build-up structure, the location shift of vibration mode’s strain energy affects the dynamic responses together with the stiffness and damping properties of joint interfaces. The thesis demonstrates that it is possible to achieve high stiffness and high damping simultaneously in materials and structures. Analysis of the vibrational strain energy distribution was found essential for the success of vibration control.

Disertacijos tikslas buvo nustatyti fizikines priežastis, ribojančias dielektrinių optinių dangų spektrinius parametrus bei jų atsparumą lazerio spinduliuotei ir pateikti įvairių jų gamybos etapų – optinių pagrindukų paruošimo dengimo procesui, optinių dangų struktūros bei dengimo technologijų optimizavimo rekomendacijas optinių komponentų gamintojams. Šiame darbe buvo atlikta komerciškai poliruotų kvarco pagrindukų visapusiška paviršiaus analize, kuri parodė, kad paviršiuje esama poliravimo medžiagų liekanų įstrigusių įvairiuose rėžiuose bei mikrotrūkiuose ir “paslėptų” po taip vadinamu Bilbio sluoksniu. Siekiant nuėsdinti šį sluoksnį ir pašalinti poliravimo medžiagų liekanas, buvo sukurta cheminio ėsdinimo HF/HNO3 tirpale metodika. Nustatyta, kad ėsdintų kvarco pagrindukų pažaidos lazerio spinduliuotei slenkstis padidėjo apie 4 kartus. Šiame darbe didelis dėmesys buvo skiriamas naujų optinių dangų modelių paieškai ir dangų formavimui, naudojant ZrO2/SiO2 medžiagų mišinius. Panaudojant metalų oksidų mišinių sluoksnius, buvo suformuotos didelio atsparumo skaidrinančios dangos ant netiesinių LBO kristalų bei didelio atspindžio periodiškai kintančio lūžio rodiklio optinės dangos ant kvarco pagrindukų. Šiame darbe buvo pasirinktas magnetroninio dulkinimo technologijos, kuri yra santykinai nauja optinių dangų industrijoje, optimizavimas. Pirma kartą pademonstruota reaktyvaus magnetroninio dulkinimo proceso valdymas, panaudojant kombinuotą reaktyviųjų dujų jutiklį. Jo pagalba buvo... [toliau žr. visą tekstą] / The main aim of this dissertation was to identify physical causes that limit optical component‘s spectral properties and resistance to laser radiation as well as to optimize the final substrate preparation procedure and coating deposition technology. In this work we report an experimental investigation of subsurface damage (SSD) in conventionally polished fused silica (FS) substrates, which are widely used in laser applications and directly influence performances of optical elements. Subsurface damages are defined as residual digs and scratches, some of which are filled with polishing slurry and covered with so-called Bielby layer (polished layer). Acid etching procedure of FS substrates was developed, which allows removing polished layer and eliminating SSD. Different durations of acid etching have been used to study laser induces damage threshold (LIDT) of FS substrates. These experiments revealed that the optimal etching time is ~1 min for a given acid concentration. LIDT of etched FS samples increased ~4 times. The LIDT in LiB3O5 (LBO) crystals coated with different types of (single AR@355 nm and triple AR@355+532+1064 nm wavelength) anti-reflective coatings was also investigated. All these coatings were produced of different oxide materials (ZrO2, Al2O3, and SiO2) and ZrO2-SiO2 mixtures by using the ion beam sputtering (IBS) deposition technique. Also, we present explorations of reactive magnetron sputtering technology for deposition of ZrO2 and Nb2O5/SiO2 mixture thin... [to full text]

The main aim of this dissertation was to identify physical causes that limit optical component‘s spectral properties and resistance to laser radiation as well as to optimize the final substrate preparation procedure and coating deposition technology. In this work we report an experimental investigation of subsurface damage (SSD) in conventionally polished fused silica (FS) substrates, which are widely used in laser applications and directly influence performances of optical elements. Subsurface damages are defined as residual digs and scratches, some of which are filled with polishing slurry and covered with so-called Bielby layer (polished layer). Acid etching procedure of FS substrates was developed, which allows removing polished layer and eliminating SSD. Different durations of acid etching have been used to study laser induces damage threshold (LIDT) of FS substrates. These experiments revealed that the optimal etching time is ~1 min for a given acid concentration. LIDT of etched FS samples increased ~4 times. The LIDT in LiB3O5 (LBO) crystals coated with different types of (single AR@355 nm and triple AR@355+532+1064 nm wavelength) anti-reflective coatings was also investigated. All these coatings were produced of different oxide materials (ZrO2, Al2O3, and SiO2) and ZrO2-SiO2 mixtures by using the ion beam sputtering (IBS) deposition technique. Also, we present explorations of reactive magnetron sputtering technology for deposition of ZrO2 and Nb2O5/SiO2 mixture thin... [to full text] / Disertacijos tikslas buvo nustatyti fizikines priežastis, ribojančias dielektrinių optinių dangų spektrinius parametrus bei jų atsparumą lazerio spinduliuotei ir pateikti įvairių jų gamybos etapų – optinių pagrindukų paruošimo dengimo procesui, optinių dangų struktūros bei dengimo technologijų optimizavimo rekomendacijas optinių komponentų gamintojams. Šiame darbe buvo atlikta komerciškai poliruotų kvarco pagrindukų visapusiška paviršiaus analize, kuri parodė, kad paviršiuje esama poliravimo medžiagų liekanų įstrigusių įvairiuose rėžiuose bei mikrotrūkiuose ir “paslėptų” po taip vadinamu Bilbio sluoksniu. Siekiant nuėsdinti šį sluoksnį ir pašalinti poliravimo medžiagų liekanas, buvo sukurta cheminio ėsdinimo HF/HNO3 tirpale metodika. Nustatyta, kad ėsdintų kvarco pagrindukų pažaidos lazerio spinduliuotei slenkstis padidėjo apie 4 kartus. Šiame darbe didelis dėmesys buvo skiriamas naujų optinių dangų modelių paieškai ir dangų formavimui, naudojant ZrO2/SiO2 medžiagų mišinius. Panaudojant metalų oksidų mišinių sluoksnius, buvo suformuotos didelio atsparumo skaidrinančios dangos ant netiesinių LBO kristalų bei didelio atspindžio periodiškai kintančio lūžio rodiklio optinės dangos ant kvarco pagrindukų. Šiame darbe buvo pasirinktas magnetroninio dulkinimo technologijos, kuri yra santykinai nauja optinių dangų industrijoje, optimizavimas. Pirma kartą pademonstruota reaktyvaus magnetroninio dulkinimo proceso valdymas, panaudojant kombinuotą reaktyviųjų dujų jutiklį. Jo pagalba buvo... [toliau žr. visą tekstą]

Transparent conductive oxides (TCOs) are key functional materials in existing and future electro-optical devices in the fields of energy efficiency, energy generation and information technology. The main application of TCOs is as thin films transparent electrodes where a combination of maximum electrical conductivity and transmittance in the visible to nearinfrared spectral range is required. However, due to the interdependence of the optical properties and the free electron density and mobility, respectively, these requirements cannot be achieved simultaneously in degenerately doped wide band-gap oxide semiconductors. Therefore, a detailed understanding of the mechanisms governing the generation of free charge carriers by extrinsic doping and the charge transport in these materials is essential for further development of high performance TCOs and corresponding deposition methods. The present work is aimed at a comprehensive investigation of the electrical, optical and structural properties as well as the elemental composition of (Al,Ga) doped ZnO and Nb doped TiO2 thin films prepared by pulsed DC reactive magnetron sputtering. The evolution of the film properties is studied in dependence of various deposition parameters through a combination of characterization techniques including Hall-effect, spectroscopic ellipsometry, spectral photometry, X-ray diffraction, X-ray near edge absorption, Rutherford backscattering spectrometry and particle induced X-ray emission. This approach resulted in the development of an alternative process control method based on the material specific current-voltage pressure characteristics of the reactive magnetron discharge which allows to precisely control the oxygen deficiency of the sputter deposited films. Based on the experimental data, models have been established that describe the room temperature charge transport properties and the dielectric function of the obtained ZnO and TiO2 based transparent conductors. On the one hand, these findings allow the prediction of material specific electron mobility limits by identifying the dominating charge carrier scattering mechanisms. On the other hand, new insight is gained into the origin of the observed transition from highly conductive to electrically insulating ZnO layers upon the incorporation of increasing concentrations of Al at elevated growth temperatures. Moreover, the Al and Ga dopant activation in ZnO have been quantified systematically for a wide range of Al concentrations and deposition conditions. A direct comparison of the Ga and Al doping efficiency demonstrates that Ga is a more efficient electron donor in ZnO. Further, it has been shown that high free electron mobilities in polycrystalline and epitaxial Nb:TiO2 layers can be achieved by reactive magnetron sputtering of TiNb alloy targets. The suppression of rutile phase formation and the control of the Nb dopant activation by fine tuning the oxygen deficiency have been identified as crucial for the growth of high quality TiO2 based TCO layers.

L’utilisation croissante de systèmes électroniques miniaturisés induit une forte demande en microsources d’énergie performantes, telles que les microbatteries au lithium. En vue d’améliorer les propriétés de l’électrolyte, nous avons étudié les propriétés électriques et thermomécaniques d’électrolytes solides de type borate de lithium. Une corrélation entre la conductivité ionique et le coefficient de dilatation thermique (CTE) a été mise en évidence pour différentes compositions de verres massifs. A partir des résultats de CTE obtenus, un modèle de prédiction basé sur les travaux de Appen permettant la détermination de ce dernier en fonction de la composition chimique a été développé. Dans un second temps, différentes techniques de préparation de cibles denses nitrurées ont été mises en œuvre afin d’abaisser le CTE de la cible et ainsi permettre son utilisation sur une plus longue durée. Par ailleurs, l’utilisation d’une cible nitrurée a également été envisagée pour augmenter la teneur en azote dans les couches minces. Finalement, des couches minces d’électrolyte de différentes compositions ont été préparées par pulvérisation cathodique (sous plasma d’argon ou d’azote pur) et ont fait l’objet d’une caractérisation chimique, structurale, électrique et thermomécanique. Le rôle bénéfique de l’azote sur la conductivité ionique des couches minces a ainsi pu être confirmé. / The growing use of miniaturized electronic devices results in a strong demand in high-performance energy microsources, such as lithium microbatteries. In order to improve electrolyte properties, we have studied the electrical and thermomechanical properties of bulk electrolyte based on lithium borate glasses. A correlation between ionic conductivity and thermal expansion coefficient has been evidenced for bulk materials. Further to CTE results, a predicting model based on studies leaded by Appen allowing a determination of CTE as a function of the chemical composition has been developed. In a second time, different preparation techniques of dense nitrated targets have been implemented in order to decrease their CTE and to allow their use for a longer period. Otherwise, nitrated targets have also been considered to increase the nitrogen content in thin films. Finally, electrolyte thin films of different compositions have been prepared by rf magnetron sputtering (under pure argon or nitrogen gas) and have been chemically, structurally, electrically and thermomecanically characterized. The favorable influence of nitrogen on the ionic conductivity of thin films has been confirmed.

Submitted by Wagner Henrique Rabelo (wagner144@bol.com.br) on 2018-07-26T20:18:44Z No. of bitstreams: 1 MESTRADO - WAGNER RABELO - VERSÃO FINAL.pdf: 3489307 bytes, checksum: 98e6a7b1b48eed69e255358e3a62fdd9 (MD5) / Approved for entry into archive by Lucilene Cordeiro da Silva Messias null (lubiblio@bauru.unesp.br) on 2018-07-30T12:45:51Z (GMT) No. of bitstreams: 1 rabelo_mh_me_bauru.pdf: 3537069 bytes, checksum: 6434660c8d96cc051a92066c85136ebc (MD5) / Made available in DSpace on 2018-07-30T12:45:51Z (GMT). No. of bitstreams: 1 rabelo_mh_me_bauru.pdf: 3537069 bytes, checksum: 6434660c8d96cc051a92066c85136ebc (MD5) Previous issue date: 2018-05-28 / O avanço das técnicas de deposição de filmes finos sobre as superfícies dos materiais tem permitido agregar valor e dar novas funcionalidades aos produtos. Atualmente, os filmes finos de óxido de estanho dopado com índio (ITO) têm encontrado grande aplicação no mercado. Entretanto, devido à pouca disponibilidade do índio na natureza e aos altos custos envolvidos na sua aquisição, elementos alternativos estão sendo estudados para sua substituição. Nesse contexto, destaca-se o óxido de zinco dopado com alumínio (AZO) como um promissor substituto, devido às características de elevada transmissividade, baixa resistividade e band gap da ordem de 3,37 eV, que permitem sua aplicação na síntese de filmes finos semicondutores. Com base no exposto, neste trabalho, foi projetado e desenvolvido o protótipo de uma fonte amplificadora de potência (FAP) de corrente alternada (AC) em baixa frequência, operando entre 15 a 40 kHz, responsável por iniciar e sustentar o campo elétrico utilizado para a geração do plasma. Esta FAP foi utilizada para a deposição de filmes finos de (AZO) por meio da técnica de magnetron sputtering. A análise das características morfológicas, ópticas e elétricas dos filmes de AZO produzidos neste estudo resultaram em uma transmitância superior a 80%, energia de band gap de 3,82 eV, e resistividade de 1,46.10-3 .cm, permitindo concluir que o filme produzido se comporta como um TCO (óxido transparente condutivo). A comparação desses resultados com trabalhos disponíveis na literatura, permite concluir que a fonte amplificadora de potência desenvolvida nesta dissertação possibilita a obtenção de filmes finos de AZO com condutividade e transparência superiores àqueles produzidos com fontes operando em radiofrequência, técnica atualmente disponível e amplamente utilizada no mercado. / The development of thin films deposition techniques allows to increase value and give new features to the materials. Currently, indium doped zinc oxide (ITO) is widely used in the market. However, due to the low availability of the indium in the nature and the high costs involved on its acquisition, alternative elements are being studied for its replacement. Aluminum doped zinc oxide (AZO) stands out as a promising substitute, mainly because of its characteristics, such as high transmissivity, low resistivity and band gap value of 3.37 eV. That allow the application of AZO in the synthesis of thin films semiconductors. In this work, it was developed a prototype of a plasma power source amplifier (FAP) to operate in alternating current (AC) and low frequency (15 - 40 kHz), responsible for initiating and sustaining the electric field used for plasma generation. This FAP was used to deposit AZO thin films by the technique of magnetron sputtering. The analysis of the morphological, optical and electrical characteristics of the AZO films produced in this study resulted in more than 80% transmittance, band gap energy value of 3,82eV, and resistivity of 1,46.10-3 .cm. The thin films synthetized was classified as transparent conductive oxide (TCO). The comparison of these results with the characteristics of similar films avaiable in the bibliography, allows to conclude that the power amplifier source developed in this dissertation makes it possible to obtain thin films of AZO with conductivity and transparency superior to those produced with RF magnetron sputtering, technique currently available and widely used in the market.

Transition metal carbides have great industrial importance with a wide area of applications. Unlike many ceramic materials which can be produced from raw materials found in nature, the refractory carbides generally do not exist in the natural state. Synthesis of these carbides is costly and exacting. Sputtered coatings of the refractory metal carbides are of great interest for applications where hard wear-resistant materials are desired. Understanding how the experimental conditions affect the microstructure and properties in reactive sputtering deposition process is still an area of intense research activity. Reactively sputtered zirconium carbide thin films were grown on (100) silicon substrate and the influence of substrate temperature on the properties of the films were investigated. The substrate temperature was varied from ambient to 500°C and partial pressures of the sputter gas and reactive gas (argon and methane) were optimised to obtain crystalline films. Structural characteristics showed that the films exhibit nanocomposite structure consisting of ZrC nanocrystallites embedded in amorphous carbon typically at lower growth temperature (TS < 300°C), and at higher growth temperatures film were highly textured. In addition, Films deposited at 325 °C showed a distinct increase in FWHM which had considerable effect on the mechanical properties of the film. Maximum hardness of 24.8 GPa was seen at 325ºC. The changes in atomic bonding structures, their relative fractions with respect to substrate temperature were discussed. We also report superhard nanocrystalline nanocomposite NbC thin film deposited on Si (100) under 500˚C growth temperature via reactive magnetron sputtering. The pronounced nano hardness and modulus value of 42 GPa and 267 GPa at 40/60 C/Nb ratio were found to be strongly dependent on the grain size and higher percentage of carbide content. HRTEM studies further confirm the formation of nanocomposite structure with nanocrystalline grains embedded in amorphous matrix. The influence of vapour incidence angle (α= 0˚ to 75˚) on optimized ZrC and NbC thin films were investigated by depositing films in Oblique angle deposition geometry (OAD). The anisotropic growth rate of crystallographic planes and the mechanism of development of micro structural features in OAD of carbide films have been investigated. XRD and pole figure measurements indicated that the films grown at higher growth temperatures (800°C) exhibited higher degree of preferred orientation coupled with larger crystallite size whereas the films deposited at room temperature displayed random polycrystalline nature. The strong increase in porosity with increase in deposition angle with distinctly separated nanometer sized columns resulted in lowering of hardness and reduced modulus value. The film with zero incidence angle exhibited a maximum hardness and reduced modulus of 28 GPa and 223 GPa respectively. On the other hand, NbC films deposited with OAD, remained to be polycrystalline in nature with less intense peaks and also exhibited loss of preferential orientation indicating lower crystal quality with increase in vapor deposition angle. It is apparent that variation in crystallographic texture coupled with sculptured nanostructures are solely material dependent properties. Nano metric modulated ZrC/NbC superlattice multilayer structure performance has been evaluated for structural stability and hardness enhancement. Multilayers present superlattice effect in XRD patterns, which are attributed to the precise periodical stacking of crystalline monolayers also confirmed by cross section FESEM. X-ray photoelectron spectroscopy depth profile analysis was performed to get information on chemical composition of modulated layers and also to get an insight on the interface region. Hardness and modulus value of 43.2 GPa and 272 GPa was observed which is higher than individual monolayers response to mechanical loading. The enhanced hardness is possibly due to the inhibition of dislocation motion along the interface and also due to strain effects at the interface.

This diploma thesis aims to optimalization the process of magnetron sputtering and creating of thin layers for use in advanced oxidation processes. During the work was created range of TiOx layers. For this process was used physical method of sputtering called PVD. The photocatalytic activity of the deposited films was tested by degradation of organic dyes Acid Orange 7. Furthermore, the layer was analyzed on surface morphology (SEM) and the layer thickness (profilometry). Study of created layers was focused on the link between the characteristics of each layer, deposition parameters and photocatalysis properties. Based on these results, the layers were applied in a system using AOP for the decomposition of organic substances. The first chapter is devoted to a summary of existing knowledge of photocatalysis and its principles. Another chapter is devoted to the theory and methods of applying thin layers and summary of knowledge of the low-pressure discharges. In the exprimental section there are described various components of the apparatus. Furthermore, the experimental part of the work focuses on the analysis of the optimization process of applying thin layers on titanium oxide. The last chapter of the thesis contains the results of the experiments on the basis of is designed another research progress of this issue.