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The purpose of this thesis is to outline the research undertaken into the synthesis of metal chalcogenide nanomaterials followed by their behavior of in diverse thermodynamic conditions. This thesis will focus on the research of novel routes to metal chalcogenides, especially CdS, PbS and PbSe. An effort was made in order to improve existing techniques by combining knowledge from diverse fields. Instabilities in nanoparticles and related behaviors, e.g. tendency to grow in specific shapes, aggregate and coalesce, were the other focusing point of this thesis. This thesis is divided into five main chapters. The first chapter introduces nanomaterials and their potential applications. An emphasis is made on the synthetic techniques to nanomaterials and their properties. Chapter two describes the synthetic approaches that were investigated during this work. Soft-hydrothermal and microwave-assisted hydrothermal routes to nanoparticles will be described. Chapter three focuses on the formation of stable nano-shapes different than the bulk-shape for PbS and PbSe nanocrystals. Their ability to self-organise on an amorphous substrate is also presented. Chapter four describes the research undertaken by transmission electron microscopy, on the coalescence of nanocrystals. Chapter five contains detailed descriptions of the experiments that were involved during this work. A general conclusion is then followed by appendixes that contain extra-information related to this thesis.

Les chalcogénures sont des matériaux très prometteurs pour des applications dans divers domaines, comme l’enregistrement et la transmission des données, l’optique intégrée, les capteurs ou la médecine. Ceci est dû à leurs propriétés exceptionnelles, en termes de transparence dans l’infrarouge, effets photo-induits, grande solubilité pour les terres rares, ou contraste élevé des paramètres électriques et optiques lors d’un changement de phase. Pour beaucoup de ces applications, les chalcogénures doivent se présenter sous forme de couches minces. Une méthode efficace et flexible pour obtenir de telles couches est le dépôt par ablation laser (PLD).Dans cette thèse nous avons entrepris une étude systématique sur l’influence de divers paramètres, comme la longueur d’onde, la durée de l’impulsion ou la fluence du laser, la pression de dépôt et la distance cible-substrat, sur les propriétés des couches minces déposées. Deux familles de composés ont été étudiées : (GeTe)x(Sb2Te3)1-x (avec x = 0, 1/3, 1/2, 2/3, 1) et GaLaS (pur ou dopé avec des terres rares – Er et Pr). Une étude en spectroscopie optique d’émission a été également effectuée afin d’explorer la dynamique et l’énergétique du plasma créé par ablation laser. Les propriétés des couches minces ont été caractérisées par microscopie optique et électronique, profilométrie, diffraction de rayons X, spectroscopie Raman, ellipsométrie etc. Les principaux résultats indiquent de meilleures propriétés pour les couches déposées à faible longueur d’onde, courte durée d’impulsion et fluence modérée. Ils ouvrent la voie vers l’optimisation du processus PLD pour la croissance de couches minces de chalcogénures de manière contrôlée. / Chalcogenides are among the most promising materials for applications in various fields, like data storage and transmission, integrated optics, bio- and chemical-sensing, or medicine. This is due to their outstanding properties, in terms of wide infrared transparency, photo-induced effects, high rare-earth solubility or high contrast in electrical and optical parameters upon phase transformation. For many of these applications, processing of chalcogenides in form of thin films with required chemical composition and appropriate physical properties is necessary. Pulsed Laser Deposition (PLD) is one of the most efficient and flexible methods for the preparation of such multicomponent layers.In this thesis we performed a systematic study on the influence of various PLD parameters, like laser wavelength, pulse duration and fluence, background pressure and target-substrate distance, on the properties of deposited thin films. Two families of chalcogenide compounds were explored: (GeTe)x(Sb2Te3)1-x (with x = 0, 1/3, 1/2, 2/3, 1) and GaLaS (pure or doped with Er and Pr rare earths). Additionally, a time- and space-resolved optical emission spectroscopy study was performed in order to characterize the dynamics and energetics of the laser ablation plasma plume. The properties of the thin films were investigated by specific methods, as optical and electronic microscopy, profilometry, X-ray diffraction, Raman spectroscopy, ellipsometry etc. The main results indicate better properties for samples deposited at lower wavelength, short pulse duration and moderate fluence. They open the way for the optimization of the PLD process for chalcogenide thin film growth in a controlled manner.