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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
11

Plonųjų dielektrinių sluoksnių optinių ir fizinių savybių tyrimas bei jų formavimo technologijų optimizavimas / Investigation of optical and physical properties of dielectric thin films and optimization of their deposition technologies

Juškevičius, Kęstutis 12 September 2014 (has links)
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]
12

Investigation of optical and physical properties of dielectric thin films and optimisation of their deposition technologies / Plonųjų dielektrinių sluoksnių optinių ir fizinių savybių tyrimas bei jų formavimo technologijų optimizavimas

Juškevičius, Kęstutis 12 September 2014 (has links)
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]
13

Funkční tenké vrstvy pro aplikace využívající pokročilé oxidační procesy / Functional thin films for applications using advanced oxidation processes

ŠRAM, Vlastimil January 2013 (has links)
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.
14

Deposição e caracterização de filmes finos TaA1N por magnetron sputtering reativo / Deposition and characterization of TaA1N thin films by reactive magnetron sputtering

Oliveira, Givanilson Brito de 03 March 2017 (has links)
Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / Ta-Al-N thin films were prepared using reactive magnetron sputtering, in order to verify the influence of the aluminum content on the crystalline structure, hardness and oxidation resistance. The samples were characterized by Grazing Incidence X-ray Diffraction (GIXRD), Energy Dispersive Spectroscopy (EDS), Rutherford Backscattering Spectrometry (RBS), nanohardness analysis and oxidation tests at 500°C, 600°C and 700°C. First, it was necessary to define deposition parameters of stoichiometric TaN with face centered cubic structure. From this, TaAlN thin films were prepared and present at concentration of 2, 5, 7, 14, 24 and 41 at.%. The crystal phase for the TaAlN films was only present with addition up to 5 at.%, increasing the Al concentration the coatings will tend to be amorphous. From the SEM analysis was possible to observe the surface of the film after oxidation, all thin films showed irregularities, however the amount of such failures was lower in samples with low aluminum content. Moreover, the addition of aluminum does not result in significant gains for oxidation resistance. The highest hardness value obtained was 29 GPa for the sample containing 14 at.%. / Filmes finos de Ta-Al-N foram depositados por magnetron sputtering reativo, com o intuito de verificar a influência da variação do teor de alumínio na estrutura cristalina, na dureza e na resistência à oxidação desse revestimento. As amostras foram caracterizadas por Difração de Raios X em ângulo rasante (GAXRD), Microscopia Eletrônica de Varredura (MEV), Espectroscopia de Energia Dispersiva (EDS), Espectroscopia por Retroespalhamento Rutherford (RBS), análises de nanodureza e testes de oxidação a temperaturas de 500°C, 600°C e 700°C. Primeiro foi necessário definir os parâmetros de deposição de filmes finos de TaN estequiométrico e com estrutura cubica de face centrada. A partir disso, filmes finos de TaAlN foram depositados e apresentaram concentração de 2, 5, 7, 14, 24 e 41 at.% de Al. A fase cristalina obtida para os filmes de TaAlN se apresentou constate com a adição de até 5 at.% de Al, com o aumento da concentração de Al o filme passa a ter uma tendência a ser amorfo. A partir das análises de MEV foi possível observar a superfície dos filmes após a oxidação, todos os filmes apresentaram irregularidades na superfície, entretanto a quantidade dessas falhas foi menor nas amostras com menores concentrações de alumínio. Além disso, a adição de alumínio não trouxe ganhos significativos para a resistência à oxidação desse revestimento. O maior valor de dureza obtido foi de 29 GPa para as amostras contendo 14 at.%.
15

Etude des transferts d’énergie plasma/surface dans différents régimes de pulvérisation magnétron / Study of the energy flux during different regimes of magnetron sputtering

El Mokh Halloumi, Mariem 21 December 2016 (has links)
Pour un bon contrôle du procédé de dépôt par pulvérisation magnétron et donc des propriétés des films déposés, une meilleure connaissance des processus de pulvérisation d’une part, et de croissance du film d’autre part est nécessaire. Une façon de mettre en évidence les différents mécanismes impliqués consiste à étudier les transferts d’énergie plasma/surface en temps réel pendant le procédé. Depuis une dizaine d’année, un outil de diagnostic permettant de mesurer directement l’énergie transférée, appelé ‘fluxmètre’ ou HFM (pour Heat Flux Microsensor), a été développé au GREMI. Il est basé sur l’insertion d’une thermopile dans un système adapté aux enceintes plasma basse pression. Bien que ce capteur de flux constitue un très bon outil de contrôle, son couplage avec d’autres diagnostics de la phase gazeuse (spectromètre de masse, spectroscopie d’émission, analyseur d’énergie etc.) et de caractérisation des films déposés (MEB, DRX, RBS,…) est nécessaire pour avoir une analyse complète du régime étudié. Pendant cette thèse, le fluxmètre a été principalement utilisé pour l’étude de trois régimes particuliers de pulvérisation magnétron en mode DC (Courant Continu); la pulvérisation en condition réactive, la pulvérisation d’une cible magnétique et la pulvérisation d’une cible chaude. Ce travail a permis de mettre en évidence des transitions de régimes dans le cas de la pulvérisation en mode réactif (oxydemétal) et à partir d’une cible magnétique (Ferro-paramagnétique). De plus, lorsqu’une cible monte en température, elle émet un rayonnement IR qui peut être absorbé avec plus ou moins d’efficacité par le film en cours de croissance. Les expériences menées dans le cadre de cette thèse ont contribué à l’étude de l’influence que cette contribution énergétique, différente de celle des processus collisionnels (condensation des atomes pulvérisés, interaction avec les ions, électrons etc.) peut avoir sur les films synthétisés. / For a good control of the magnetron sputtering process and therefore of the properties of the deposited films, a better knowledge of the sputtering processes on the one hand and the growth of the film on the other hand is necessary. One way to demonstrate the different mechanisms involved is to study the plasma / surface energy transfers in real time during the process. For the last ten years, a diagnostic tool has been developed at GREMI to directly measure the transferred energy, called fluxmeter, or HFM (for Heat Flux Microsensor). It is based on the insertion of a thermopile in a system suitable for low pressure plasma reactors. Although this flux sensor is a very good control tool, its coupling with other diagnoses of gas phase (mass spectrometer, emission spectroscopy, energy analyzer etc.) and characterization of deposited films (SEM , DRX, RBS, ...) is necessary to have a complete analysis of the studied regime. During this thesis, the fluxmeter was mainly used for the study of three particular regimes of magnetron sputtering in DC (Continuous Current) mode; the sputtering in a reactive condition, the sputtering of a magnetic target, and the sputtering of a hot target. Transitions of regimes in the case of the reactive sputtering (oxide-metal) and the magnetic target (Ferro-paramagnetic) was studied. In addition, when he target emperature rises, it emits IR radiation that can be absorbed with more or less efficiently by the growing film. The experiments carried out in this thesis contributed to the study of the influence of this energy contribution, different from the collisional processes (condensation of atomized atoms, interaction with ions, electrons etc.) can have on the films Synthesized.
16

Otimização das propriedades estruturais de filmes de nitreto de alumínio visando sua aplicação como material piezoelétrico. / Structural properties optimization of aluminum nitride films aiming their application as piezoelectric material.

Rubens Martins Cunha Junior 01 June 2015 (has links)
Neste trabalho é apresentado um estudo sobre a produção e caracterização do nitreto de alumínio (AlN) obtido pela técnica de r.f. Magnetron Sputtering reativo. Aqui reportamos o efeito dos parâmetros de deposição, como densidade de potência de r.f., temperatura e pressão de processo nas propriedades estruturais, morfológicas e elétricas dos filmes de AlN obtidos. Foram realizados estudos sobre os modos vibracionais, pela técnica de espectroscopia de infravermelho por transformada de Fourier (FTIR), das orientações cristalográficas por difração de raios X e da morfologia da superfície pela técnica de microscopia de força atômica (AFM). Estes estudos nos permitiram produzir filmes finos de AlN com uma alta orientação na direção cristalográfica [002] com uma potência de r.f. de 1,23 W/cm2 , uma temperatura de deposição de 200°C e uma pressão de processo de 2 mTorr. Este estudo nos permitiu fabricar filmes de AlN com alta orientação [002] à temperatura ambiente a partir de um alvo de Al. O coeficiente piezoelétrico d33 variou de aproximadamente 4 a 6 pm/V e o d31 2 a 3 pm/V para filmes cristalinos e d33 3 pm/V e d31 1,5 pm/V para filmes amorfos. Os coeficientes piezoelétricos d33 and d31 foram estimados pelo método capacitivo proposto por Mahmoud Al Ahmad and Robert Plana, através da variação das dimensões geométricas induzidas pelo campo elétrico aplicado. / In this work we present a study about the production and characterization of aluminum nitride (AlN) obtained by r.f. Reactive Magnetron Sputtering. Here we report the effect of the deposition parameters, such as r.f. power density, and deposition temperature and pressure, on the morphological, structural and electrical properties of the obtained AlN thin films. In this work we have performed studies concerning the vibrational modes by Fourier Transform Infrared Absorption technique (FTIR), the crystallographic orientations by X-ray diffraction and the surface morphology by Atomic Force Microscopy (AFM). This study allowed us to produce high oriented [002] AlN thin films with a r.f. power density of 1.23 W/cm2, a deposition temperature of 200ºC and a process pressure of 2 mTorr. This study allowed us to produce high oriented [002] AlN thin films at room temperature from a pure Al target. The piezoelectric coefficient d33 was around 4 to 6 pm/V and d31 2 to 3 pm/V to crystalline films and d33 3 pm/V and d31 1.5 pm/V amorphous ones. d33 and d31 piezoelectric coefficients were estimated by the capacitive method proposed by Mahmoud Al Ahmad and Robert Plana, through its geometrical dimensions variation.
17

Otimização das propriedades estruturais de filmes de nitreto de alumínio visando sua aplicação como material piezoelétrico. / Structural properties optimization of aluminum nitride films aiming their application as piezoelectric material.

Cunha Junior, Rubens Martins 01 June 2015 (has links)
Neste trabalho é apresentado um estudo sobre a produção e caracterização do nitreto de alumínio (AlN) obtido pela técnica de r.f. Magnetron Sputtering reativo. Aqui reportamos o efeito dos parâmetros de deposição, como densidade de potência de r.f., temperatura e pressão de processo nas propriedades estruturais, morfológicas e elétricas dos filmes de AlN obtidos. Foram realizados estudos sobre os modos vibracionais, pela técnica de espectroscopia de infravermelho por transformada de Fourier (FTIR), das orientações cristalográficas por difração de raios X e da morfologia da superfície pela técnica de microscopia de força atômica (AFM). Estes estudos nos permitiram produzir filmes finos de AlN com uma alta orientação na direção cristalográfica [002] com uma potência de r.f. de 1,23 W/cm2 , uma temperatura de deposição de 200°C e uma pressão de processo de 2 mTorr. Este estudo nos permitiu fabricar filmes de AlN com alta orientação [002] à temperatura ambiente a partir de um alvo de Al. O coeficiente piezoelétrico d33 variou de aproximadamente 4 a 6 pm/V e o d31 2 a 3 pm/V para filmes cristalinos e d33 3 pm/V e d31 1,5 pm/V para filmes amorfos. Os coeficientes piezoelétricos d33 and d31 foram estimados pelo método capacitivo proposto por Mahmoud Al Ahmad and Robert Plana, através da variação das dimensões geométricas induzidas pelo campo elétrico aplicado. / In this work we present a study about the production and characterization of aluminum nitride (AlN) obtained by r.f. Reactive Magnetron Sputtering. Here we report the effect of the deposition parameters, such as r.f. power density, and deposition temperature and pressure, on the morphological, structural and electrical properties of the obtained AlN thin films. In this work we have performed studies concerning the vibrational modes by Fourier Transform Infrared Absorption technique (FTIR), the crystallographic orientations by X-ray diffraction and the surface morphology by Atomic Force Microscopy (AFM). This study allowed us to produce high oriented [002] AlN thin films with a r.f. power density of 1.23 W/cm2, a deposition temperature of 200ºC and a process pressure of 2 mTorr. This study allowed us to produce high oriented [002] AlN thin films at room temperature from a pure Al target. The piezoelectric coefficient d33 was around 4 to 6 pm/V and d31 2 to 3 pm/V to crystalline films and d33 3 pm/V and d31 1.5 pm/V amorphous ones. d33 and d31 piezoelectric coefficients were estimated by the capacitive method proposed by Mahmoud Al Ahmad and Robert Plana, through its geometrical dimensions variation.
18

Etude de revêtements photocatalytiques à base de dioxyde de titane nanostructuré élaborés par pulvérisation cathodique magnétron en condition réactive / Photocatalytic coatings based on nanostructured titanium dioxide prepared by reactive magnetron sputtering

Sayah, Imane 17 December 2014 (has links)
Le développement de photocatalyseurs en couches minces supportées constitue un intérêt majeur autorisant une séparation efficace des produits de réaction, en dépit d’une réduction de leur surface spécifique par rapport à des nanopoudres du même matériau. La synthèse de revêtements de TiO2 par pulvérisation cathodique magnétron en condition réactive fait l’objet de recherches intensives. Cette technique permet de contrôler, à travers les paramètres d’élaboration, la structure et les propriétés physicochimiques et photocatalytiques des revêtements.Afin de s’affranchir de la contamination du catalyseur par le sodium du verre lors de traitements en température ou lors de recuits de couches déposées à l’ambiante, une barrière de diffusion en SiNx est intercalée et son épaisseur est fixée pour la suite de l’étude. Différentes couches de TiO2 ont été élaborées à haute pression dans un réacteur doté d’un système de contrôle en boucle fermée basé sur la spectroscopie d’émission optique. L’effet de la cristallisation in situ à différentes températures sur les différentes propriétés des revêtements TiO2 a été étudié et les propriétés de ces derniers ont été comparées à celles des échantillons synthétisés sur des substrats froids et recuits ex situ aux mêmes températures.Enfin, des premiers travaux portant sur l’influence de l’introduction de l’argent en différentes teneurs sur l’efficacité photocatalytique sous lumière visible des couches de TiO2 cristallisées in situ et ex situ sont présentés. / The development of supported photocatalysts thin films is of major interest allowing an efficient separation of the reaction products, in spite of their specific area reduction compared to nanometric scale powders. The synthesis of TiO2 coatings by reactive magnetron sputtering is the subject of intensive researches. This technique allows, trough the control of the deposition parameters, to manage the structure and the physicochemical and photocatalytic properties of the coatings. In order to hinder the sodium contamination of the catalyst from the glass substrate, either during in situ or ex situ heating of the coating, a SiNx diffusion barrier is intercalated with a fixed thickness. Different layers of TiO2 were prepared at high pressure in a reactor equipped with a closed-loop control system based on optical emission spectroscopy. The influence of the in situ crystallization at different temperatures on the properties of the TiO2 coatings was studied. These properties were compared with those of samples synthesized ex situ and at the same temperatures. Finally, first studies on the influence of silver enrichment at different contents on photocatalytic activity under visible light of TiO2 layers crystallized in situ and ex situ, are presented.
19

Synthèse par pulvérisation magnétron et caractérisation de couches minces photochromes / Synthesis by magnetron sputtering and characterization of photochromic thin films

Diop, Daouda Keïta 10 November 2016 (has links)
Ces travaux de thèse rentrent dans le cadre de l'ANR Photoflex (2013-2016) qui vise à mettre au point une technologie d'impression laser sans contact, pour créer des motifs actualisables ou permanents à caractère unique sur tout type de support, en particuliers des supports souples. Nous rapportons la synthèse par technique de pulvérisation magnétron en mode réactif et à température ambiante de films minces nanocomposites photochromes constitués de nanoparticules d'Ag entre deux couches nanoporeuses de TiO2. Ces films sont déposés sur des substrats souples tels qu'un plastique transparent (PET) et un papier diffusant. Nous montrons que lorsque le TiO2 est élaboré en régime de pulvérisation élémentaire, le film nanocomposite est coloré en raison de la présence de nanoparticules d'Ag métalliques induisant une résonance de plasmons de surface localisés dans le visible. En revanche, en régime de pulvérisation composite, le film nanocomposite est incolore car l'Ag s'oxyde lors de son recouvrement par le TiO2. Nous avons démontré que les échantillons incolores peuvent se colorer sous insolation laser UV (244 nm) dû à la réduction de l'Ag oxydé puis à la croissance de nanoparticules d'Ag métalliques par coalescence ou par mûrissement d'Ostwald. De plus, l'insolation laser visible (647 nm) à de faibles éclairements (quelques W.cm-2) de ce type de film ou des films initialement colorés donne lieu à des changements morphologiques des nanoparticules d'Ag qui modifient l'absorbance du film et entraînent une modification de la coloration de l'échantillon. Nous avons étudié l'influence des conditions de dépôt (épaisseur de la couche de recouvrement des nanoparticules, épaisseur de la sous-couche de TiO2, quantité d'Ag, temporisation après dépôt d'Ag, traitement plasma des nanoparticules d'Ag, multicouches) afin d'optimiser les effets de photochromisme en amplitude et en vitesse. Tous les mécanismes de photochromisme sont répétables durant des processus cycliques d'insolation UV/Visible. Pour de forts éclairements en laser visible (plusieurs dizaines de kW.cm-2), nous avons observé sur des films nanocomposites déposés sur verre, des changements de couleurs dépendants de la direction de polarisation du faisceau sonde, liés à la croissance thermique et à l'auto-organisation de l'Ag selon un réseau périodique de chaînes de nanoparticules. Contrairement aux faibles éclairements, les couleurs photo-induites sont permanentes et présentent un caractère dichroïque. Cette étude ouvre des perspectives intéressantes en termes d'applications, notamment pour l'authentification et la traçabilité de produits manufacturés, le stockage de données, les nouvelles générations de datamatrix, etc. / These thesis works are within the framework of the ANR Photoflex (2013-2016), which aims to develop a contactless laser printing technology, in order to create updatable or permanent patterns of unique character on any types of supports, especially flexible supports. We report on a reactive magnetron sputtering-based deposition method to synthesize, at room temperature, photochromic nanocomposite thin films consisting of Ag nanoparticles sandwiched between nanoporous TiO2 layers. These films are deposited on flexible substrates such as a transparent plastic (PET) and a diffusing paper. We show that when the TiO2 is elaborated in the metallic sputtering mode, the nanocomposite film is colored due to the formation of metal Ag nanoparticles inducing a localized surface plasmon resonance in the visible range. In contrast, in the compound sputtering mode, the nanocomposite film is colorless because the Ag nanoparticles are oxidized during their capping by the TiO2. We have demonstrated that the colorless samples can be colored under UV laser irradiation (244 nm) due to the reduction of oxidized silver, followed by the growth of metallic Ag nanoparticles by coalescence or Ostwald ripening. Moreover, visible laser irradiation at low irradiances (few W.cm-2) of the colored films gives rise to changes in the particle morphology that modifies the absorbance of the films and results in sample color changes. We have investigated the influence of the deposition conditions (capping layer thickness of nanoparticles, TiO2 buffer layer thickness, Ag amount, holding time after Ag deposition, plasma annealing of Ag nanoparticles, multilayer) in order to optimize the photochromic effects in amplitude and in speed. All the mechanisms are repeatable during UV/Visible irradiation cyclic processes. For strong visible laser irradiances (several tens of kW.cm-2), we observed on nanocomposite films deposited on glass, color changes dependent on the polarization direction of the probe beam, related to the thermal growth and to the self-organization of Ag according to a periodic grating of nanoparticle chains. Contrary to low irradiances, the photo-induced colors are permanent and have a dichroic character. This study opens up interesting possibilities in terms of applications, including authentication and traceability of manufactured products, data storage, the new generation of datamatrix, etc.
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Micro- et nanostructure des revêtements (Ti, Al)N et comportement tribologique au voisinage de la transition structurale / Micro- and nanostructure of Ti1-xAlxN thin films and wear close to the structural transition (fcc/hcp)

Pinot, Yoann 20 January 2015 (has links)
Les films de nitrures métalliques nanostructurés sont généralement utilisés comme revêtements protecteurs. Ti1-xAlxN (0 ≤ x ≤ 1) peut être considéré comme un système modèle, où TiN (cubique) et AIN (hexagonal) sont partiellement miscibles. L’élaboration par dépôt physique en phase vapeur donne au film une microstructure colonnaire complexe composée de phase métastable pouvant cohabiter avec des précipités localisés aux joints de grains. Une haute dureté et une grande résistance à l’oxydation sont observées pour un maximum d’atomes de Ti substitué par des atomes de Al en réseau cubique. Les conditions de dépôt et la composition jouent un rôle majeur sur la substitution des éléments métalliques (Ti ,Al). Nous avons préparé deux séries de films déposés par pulvérisation cathodique magnétron réactive à partir de cibles TiAl compartimentées et frittées. La micro- et nanostructure des films ont été analysées par Diffraction, Spectroscopie d’Absorption des rayons X et Microscopie Electronique à Transmission. L’usure des revêtements a été étudiée par microtribologie. Nous observons pour les films riches en Ti (x < 0,5) des directions de croissances [200]c et [111]c, caractéristiques d’un réseau cubique. Tandis que, les films riches en Al (x > 0,7) présentent une croissance de domaines bien cristallisés suivant la direction [002]h du réseau hexagonal. De plus, nous avons mis en évidence l’apparition de la transition cubique / hexagonal à des teneurs en Al plus élevée pour les films issus de cible frittée. Ces films montrent une meilleure résistance à la fissuration et à l’usure que ceux déposés à partir de cible compartimentées. / Ti1-xAlxN (0 ≤ x ≤ 1) is considered as a model system, where TiN (fcc) and AlN (hcp) do not mix over the whole composition range due to their low miscibility. However, the physical vapour deposition (PVD) allows achieving metastable phases of Ti1-xAlxN, where Al atoms are partially substituting for Ti in fcc lattice. Ti1-xAlxN coatings exhibit high hardness and oxidation resistance for the maximum Al substituted to Ti in fcc lattice (about x=0.6). The proportion of grain boundaries and the limit solubility play a major role on the mechanical properties and resistance to wear of the coatings. Several techniques are employed to investigate two sets of Ti1-xAlxN thin films deposited by magnetron reactive sputtering from two types of metallic targets onto Si (100). Lattice symmetry of crystallised domains and columnar growth structure of the films are characterized by X-ray diffraction (XRD) and electron microscopy (TEM, HRTEM). Several local probes such as X-ray absorption fine structure (XAFS), diffraction anomalous fine structure (DAFS) and Electron Energy Loss Spectroscopies (EELS) which are very sensitive to the symmetry of the atomic sites either octahedral for fcc lattice or tetrahedral for hcp one are carried out. For Ti-rich films (x < 0.5), the competitive growth of cubic domains between [200]c and [111]c is observed. For Al-rich films (x > 0.7) have a domain growth well crystallized in the direction [002]h the hexagonal lattice. In addition, the cubic / hexagonal transition in Al contents higher is observed for films from sintered target. These films show better wear resistance than those deposited from target compartmentalized.

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