This thesis reflects two advances in atomic force microscopy. The first half is a new lateral force calibration procedure, which, in contrast to existing procedures, is independent of sample and cantilever shape, simple, direct, and quick. The second half is a high-throughput method for processing, fitting, and analyzing force curves taken on Pseudomonas aeruginosa bacteria in an effort to inspire better care for statistics and increase measurement precision.

COSTA, Erivelton Façanha da. Estudo das propriedades mecânicas de misturas asfálticas por microscopia de força atômica. 2011. 131 f. Tese (Doutorado em Física) - Programa de Pós-Graduação em Física, Departamento de Física, Centro de Ciências, Universidade Federal do Ceará, Fortaleza, 2011. / Submitted by Edvander Pires (edvanderpires@gmail.com) on 2015-05-05T21:11:07Z No. of bitstreams: 1 2011_tese_efcosta.pdf: 9690898 bytes, checksum: 515b97b02ebfcf8c3652b217cd15491b (MD5) / Approved for entry into archive by Edvander Pires(edvanderpires@gmail.com) on 2015-05-07T16:57:29Z (GMT) No. of bitstreams: 1 2011_tese_efcosta.pdf: 9690898 bytes, checksum: 515b97b02ebfcf8c3652b217cd15491b (MD5) / Made available in DSpace on 2015-05-07T16:57:29Z (GMT). No. of bitstreams: 1 2011_tese_efcosta.pdf: 9690898 bytes, checksum: 515b97b02ebfcf8c3652b217cd15491b (MD5) Previous issue date: 2011 / The rheological study of asphalt binders is of great importance for determining its performance in paving construction. Usually, rheological parameters are obtained by a Dynamic Shear Rheometer (DSR). The aim of this work is to study the rheological properties of bitumen using an Atomic Force Microscope (AFM). So, a computational tool caled FVLOAD was used for imaging processing. Five kinds of mathematical models were used in order to analise the force curves colected through AFM: the slope analysis, the Young´s model, the adesion model, the FIEL model (Force Integration to Equal Limits) and the work difference model. Three samples were studied: pure bitumen 50/70, bitumem 50/70 doped with 4% of EVA and bitumem 50/70 doped with 4,5% of SBS. Very thin lms of these materials were prepared on glass slides and lead to an AFM for imaging. The area studied on the sample surface was of 50 m x 50 m. There were colected 1024 force curves for each image. The indentations were carried out in four frequencies: 0,5 Hz, 5 Hz, 14 Hz e 28 Hz. The curves colected were analyzed with the FVLOAD program and once the elastic properties were calculated, they were compared to those obtained in the Dynamic Shear Rheometer. / O estudo reológico do Cimento Asfáltico de Petróleo (CAP) é de fundamental importância para a determinação de sua performance na fabricação de estradas. Usualmente os parâmetros reológicos deste tipo de material são obtidos em ensaios dinâmicos através de um reômetro de cisalhamento. O presente trabalho tem por objetivo estudar as propriedades reológicas do CAP através da técnica de espectroscopia de força utilizando um microscópio de força atômica. Para isso, foi utilizada uma ferramenta computacional desenvolvida para o processamento das imagens de microscopia de força chamada de FVLOAD. Cinco análises foram realizadas com os dados das curvas de força: análise de slope, análise do módulo elástico ou módulo de Young, análise de adesão do filme de CAP, análise FIEL (Force Integration to Equal Limits), Work Difference e Adesão. Três amostras foram utilizadas neste estudo: CAP puro 50/70, CAP com 4% de EVA e CAP com 4,5% de SBS. Filmes dos três tipo de CAP foram confeccionados em lamínulas de vidro e levados ao microscópio de força atômica para obtenção dos dados das curvas de força sobre uma área de 50 μm x 50 μm. Para cada imagem foram coletadas 1024 curvas de força. As indentações com a sonda AFM foram executadas em quatro frequências: 0,5 Hz, 5 Hz, 14 Hz e 28 Hz. Finalizadas as aquisições de dados, estes foram processados no programa FVLOAD. Extraído o módulo elástico das amostras em cada frequência, os dados foram comparados com aqueles obtidos em ensaios dinâmicos através do reômetro de cisalhamento dinâmico.

Conselho Nacional de Desenvolvimento CientÃfico e TecnolÃgico / O estudo reolÃgico do Cimento AsfÃltico de PetrÃleo (CAP) Ã de fundamental importÃncia para a determinaÃÃo de sua performance na fabricaÃÃo de estradas. Usualmente os parÃmetros reolÃgicos deste tipo de material sÃo obtidos em ensaios dinÃmicos atravÃs de um reÃmetro de cisalhamento. O presente trabalho tem por objetivo estudar as propriedades reolÃgicas do CAP atravÃs da tÃcnica de espectroscopia de forÃa utilizando um microscÃpio de forÃa atÃmica. Para isso, foi utilizada uma ferramenta computacional desenvolvida para o processamento das imagens de microscopia de forÃa chamada de FVLOAD. Cinco anÃlises foram realizadas com os dados das curvas de forÃa: anÃlise de slope, anÃlise do mÃdulo elÃstico ou mÃdulo de Young, anÃlise de adesÃo do filme de CAP, anÃlise FIEL (Force Integration to Equal Limits), Work Difference e AdesÃo. TrÃs amostras foram utilizadas neste estudo: CAP puro 50/70, CAP com 4% de EVA e CAP com 4,5% de SBS. Filmes dos trÃs tipo de CAP foram confeccionados em lamÃnulas de vidro e levados ao microscÃpio de forÃa atÃmica para obtenÃÃo dos dados das curvas de forÃa sobre uma Ãrea de 50 μm x 50 μm. Para cada imagem foram coletadas 1024 curvas de forÃa. As indentaÃÃes com a sonda AFM foram executadas em quatro frequÃncias: 0,5 Hz, 5 Hz, 14 Hz e 28 Hz. Finalizadas as aquisiÃÃes de dados, estes foram processados no programa FVLOAD. ExtraÃdo o mÃdulo elÃstico das amostras em cada frequÃncia, os dados foram comparados com aqueles obtidos em ensaios dinÃmicos atravÃs do reÃmetro de cisalhamento dinÃmico. / The rheological study of asphalt binders is of great importance for determining its performance in paving construction. Usually, rheological parameters are obtained by a Dynamic Shear Rheometer (DSR). The aim of this work is to study the rheological properties of bitumen using an Atomic Force Microscope (AFM). So, a computational tool caled FVLOAD was used for imaging processing. Five kinds of mathematical models were used in order to analise the force curves colected through AFM: the slope analysis, the YoungÂs model, the adesion model, the FIEL model (Force Integration to Equal Limits) and the work difference model. Three samples were studied: pure bitumen 50/70, bitumem 50/70 doped with 4% of EVA and bitumem 50/70 doped with 4,5% of SBS. Very thin lms of these materials were prepared on glass slides and lead to an AFM for imaging. The area studied on the sample surface was of 50 m x 50 m. There were colected 1024 force curves for each image. The indentations were carried out in four frequencies: 0,5 Hz, 5 Hz, 14 Hz e 28 Hz. The curves colected were analyzed with the FVLOAD program and once the elastic properties were calculated, they were compared to those obtained in the Dynamic Shear Rheometer.

Cette thèse s'inscrit dans le domaine des problèmes inverses en traitement du signal. Elle est consacrée à la conception d'algorithmes de restauration et de séparation de signaux parcimonieux et à leur application à l'approximation de courbes de forces en microscopie de force atomique (AFM), où la notion de parcimonie est liée au nombre de points de discontinuité dans le signal (sauts, changements de pente, changements de courbure). Du point de vue méthodologique, des algorithmes sous-optimaux sont proposés pour le problème de l'approximation parcimonieuse basée sur la pseudo-norme l0 : l'algorithme Single Best Replacement (SBR) est un algorithme itératif de type « ajout-retrait » inspiré d'algorithmes existants pour la restauration de signaux Bernoulli-Gaussiens. L'algorithme Continuation Single Best Replacement (CSBR) est un algorithme permettant de fournir des approximations à des degrés de parcimonie variables. Nous proposons aussi un algorithme de séparation de sources parcimonieuses à partir de mélanges avec retards, basé sur l'application préalable de l'algorithme CSBR sur chacun des mélanges, puis sur une procédure d'appariement des pics présents dans les différents mélanges. La microscopie de force atomique est une technologie récente permettant de mesurer des forces d'interaction entre nano-objets. L'analyse de courbes de forces repose sur des modèles paramétriques par morceaux. Nous proposons un algorithme permettant de détecter les régions d'intérêt (les morceaux) où chaque modèle s'applique puis d'estimer par moindres carrés les paramètres physiques (élasticité, force d'adhésion, topographie, etc.) dans chaque région. Nous proposons finalement une autre approche qui modélise une courbe de force comme un mélange de signaux sources parcimonieux retardées. La recherche des signaux sources dans une image force-volume s'effectue à partir d'un grand nombre de mélanges car il y autant de mélanges que de pixels dans l'image / This thesis handles several inverse problems occurring in sparse signal processing. The main contributions include the conception of algorithms dedicated to the restoration and the separation of sparse signals, and their application to force curve approximation in Atomic Force Microscopy (AFM), where the notion of sparsity is related to the number of discontinuity points in the signal (jumps, change of slope, change of curvature).In the signal processing viewpoint, we propose sub-optimal algorithms dedicated to the sparse signal approximation problem based on the l0 pseudo-norm : the Single Best Replacement algorithm (SBR) is an iterative "forward-backward" algorithm inspired from existing Bernoulli-Gaussian signal restoration algorithms. The Continuation Single Best Replacement algorithm (CSBR) is an extension providing approximations at various sparsity levels. We also address the problem of sparse source separation from delayed mixtures. The proposed algorithm is based on the prior application of CSBR on every mixture followed by a matching procedure which attributes a label for each peak occurring in each mixture.Atomic Force Microscopy (AFM) is a recent technology enabling to measure interaction forces between nano-objects. The force-curve analysis relies on piecewise parametric models. We address the detection of the regions of interest (the pieces) where each model holds and the subsequent estimation of physical parameters (elasticity, adhesion forces, topography, etc.) in each region by least-squares optimization. We finally propose an alternative approach in which a force curve is modeled as a mixture of delayed sparse sources. The research of the source signals and the delays from a force-volume image is done based on a large number of mixtures since there are as many mixtures as the number of image pixels