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Development of Highly Resolved and Photo-Modulated Kelvin Probe Microscopy Techniques for the Study of Photovoltaic Systems Pablo Arturo Fernandez Garrillo

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Development of Highly Resolved and Photo-Modulated Kelvin Probe Microscopy Techniques for the Study of Photovoltaic Systems Pablo Arturo Fernandez Garrillo Development of highly resolved and photo-modulated Kelvin probe microscopy techniques for the study of photovoltaic systems Pablo Arturo Fernandez Garrillo To cite this version: Pablo Arturo Fernandez Garrillo. Development of highly resolved and photo-modulated Kelvin probe microscopy techniques for the study of photovoltaic systems. Materials Science [cond-mat.mtrl-sci]. Université Grenoble Alpes, 2018. English. NNT : 2018GREAY031. tel-01970171 HAL Id: tel-01970171 https://tel.archives-ouvertes.fr/tel-01970171 Submitted on 31 Jan 2019 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. THÈSE Pour obtenir le grade de DOCTEUR DE LA COMMUNAUTE UNIVERSITE GRENOBLE ALPES Spécialité : Nanophysique Arrêté ministériel : 25 mai 2016 Présentée par Pablo Arturo FERNÁNDEZ GARRILLO Thèse dirigée par Dr. Benjamin GRÉVIN, et encadrée par Dr. Łukasz BOROWIK Préparée au sein du Laboratoire d'Électronique et de Technologie de l'Information et de l’Institut Nanosciences et Cryogénie – CEA Grenoble dans l'École Doctorale de Physique Développement de techniques de microscopie Kelvin hautement résolues et photo- modulées pour l'étude de systèmes photovoltaïques Thèse soutenue publiquement le 25 Septembre 2018, devant le jury composé de : Dr. Sascha SADEWASSER INL (Praga, Portugal), Examinateur Pr. Pere ROCA i CABARROCAS LPICM, CNRS, Ecole Polytechnique, (Paris, France), Président Dr. Guillaume SCHULL IPCMS DSI (Strasbourg, France), Rapporteur Pr. Christian LOPPACHER VOIROL IM2NP, Faculté des Sciences et Techniques, (Marseille, France) Rapporteur Dr. Benjamin GRÉVIN UGA, CNRS, CEA, INAC, UMR-5819 (Grenoble, France), Directeur de thèse Dr. Łukasz BOROWIK UGA, CEA, LETI (Grenoble, France), Encadrant THESIS To obtain the degree of DOCTOR OF THE UNIVERSITY OF GRENOBLE Speciality: Nanophysics Ministerial decree: May 25, 2016 Presented by Pablo Arturo FERNÁNDEZ GARRILLO Thesis directed by Dr. Benjamin GRÉVIN, and supervised by Dr. Łukasz BOROWIK Prepared at the Laboratory of Electronics and Information Technology and the Nanoscience and Cryogenics Institute – CEA Grenoble at the Doctoral School of Physics Development of highly resolved and photo-modulated Kelvin probe microscopy techniques for the study of photovoltaic systems Thesis defended publicly on September 25, 2018, in front of the Ph.D. thesis committee composed by: Dr. Sascha SADEWASSER INL (Praga, Portugal), Member Pr. Pere ROCA i CABARROCAS LPICM, CNRS, Ecole Polytechnique, (Paris, France), President Dr. Guillaume SCHULL IPCMS DSI (Strasbourg, France), Referee Pr. Christian LOPPACHER VOIROL IM2NP, Faculté des Sciences et Techniques, (Marseille, France) Referee Dr. Benjamin GRÉVIN UGA, CNRS, CEA, INAC, UMR-5819 (Grenoble, France), Ph.D. Director Dr. Łukasz BOROWIK UGA, CEA, LETI (Grenoble, France), Supervisor “Look deep into nature, and then you will understand everything better.” Albert Einstein To my family, and especially to Susana, Luis David, Beatriz and Wintila. Abstract This thesis is directed towards the proposition and demonstration of a set of novel advanced atomic force microscopy based techniques under ultra-high vacuum conditions, enabling to map simultaneously the surface topography and the photo-carrier dynamics at the nanometre scale. In fact, by monitoring the dependence of the average surface photo-voltage measured with Kelvin probe force microscopy, as a function of the repetition frequency of a modulated excitation source, we will access the built-up and decay dynamics of the surface photo-voltage response which in turn will allows us to study the photo-carrier dynamics over a wide range of samples. In order to enable the 2-dimensional nano-imaging process, Kelvin probe force microscopy under modulated illumination measurements are acquired repeatedly over each point of a predefined grid area over the sample acquiring a set of spectroscopy curves. Then, using an automatic mathematical fit procedure, spectroscopy curves are translated into pixels of the photo-carrier dynamic time-constant images. Moreover, these set of novel techniques will be used to investigate the surface photo- voltage dynamics in several kinds of photovoltaic samples from different technological branches such as small grain polycrystalline silicon thin films, silicon nanocrystal-based third generation cells, bulk heterojunction donor-acceptor organic photovoltaics and organic- inorganic hybrid perovskite single crystal cells, discussing in each case the photo-carrier recombination process and its relation with the material’s structuration/morphology. Finally, technical aspects of these novel techniques will be discussed as well as their limitations and remaining open questions regarding results interpretation. ix x Résumé Cette thèse propose, décrit et utilise un ensemble de techniques basées sur la microscopie à force atomique sous ultravide pour la cartographie simultanée, à l'échelle nanométrique, de la topographie de surface et des dynamiques temporelles des photo-porteurs. Ainsi, en contrôlant la dépendance du photo-potentiel de surface moyen mesuré par microscopie à force de sonde Kelvin en fonction de la fréquence de répétition d'une source lumineuse externe d'excitation, le dispositif expérimental permet d’accéder aux dynamiques temporelles du photo-potentiel de surface qui, à leur tour, permettent d'étudier les dynamiques des photo-porteurs sur une large gamme d'échantillons. Afin de permettre le processus de nano- imagerie bidimensionnelle, ces mesures sont acquises de manière répétée en enregistrant des courbes spectroscopiques en chaque point d’une grille prédéfinie. En utilisant une procédure d'ajustement mathématique automatique, les dynamiques temporelles des photo-porteurs sont extraites à partir des données expérimentales. Cet ensemble de nouvelles méthodes est utilisé pour l’étude de plusieurs types d'échantillons issus de différentes technologies photovoltaïques telles que des couches minces en silicium poly-cristallin à petits grains, des cellules de troisième génération à nano cristaux de silicium, des cellules photovoltaïques organiques et des cellules à base de matériaux de structure pérovskite. Dans chaque cas, on décrit les processus de recombinaison des photo- porteurs ainsi que leur lien avec la morphologie et la structuration du matériau. Enfin, les aspects techniques de ces nouvelles méthodes d’analyse sont présentés, ainsi que leurs limites, notamment celles concernant l'interprétation des résultats. xi xii Contents Abstract ..................................................................................................................................... ix Résumé ...................................................................................................................................... xi Contents ................................................................................................................................. xiii List of Figures ........................................................................................................................ xvii Notations ................................................................................................................................. xxi 1 | Introduction ........................................................................................................................... 1 1.1 Thesis Outline ............................................................................................................. 8 References ............................................................................................................................ 10 2 | Photovoltaics ....................................................................................................................... 13 2.1 Context ........................................................................................................................... 13 2.2 Physics of classic solar cells: The case of silicon and other inorganic photovoltaics technologies ......................................................................................................................... 16 2.3 Organic photovoltaics .................................................................................................... 26 2.4 Perovskite photovoltaics ................................................................................................ 32 2.5 Characterization methods ............................................................................................... 35 Conclusion ........................................................................................................................... 37 References ............................................................................................................................ 39 3 | Scanning probe microscopy techniques ............................................................................. 45 3.1 Context ........................................................................................................................... 46 3.2 Nanotechnology ............................................................................................................
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