Éditeur(s) : HAL CCSD
Résumé : The presence of biological matter (biofilms) in deep geological sites for storage of, for instance, toxic elements or groundwater in aquifers was clearly proved. That biomass triggers physical and chemical processes which greatly modify the durability and the sustainability of the sites. These processes, mainly from oxidative/reductive reactions, are poorly understood. This is mainly due to the fact that former studies were done at the macroscopic level far away from the micrometric scale where relevant processes induced by bacteria take place. Investigations at microscopic level are needed. Thus, we developed an experimental set-up based on the combined use of optical microscopy (transmission), atomic force microscopy (AFM) and electrical and electro-chemical AFM microscopy (EC_AFM) in order to get simultaneous information on topographic and electro-chemical processes. The first highly sensitive step was to use AFM with biological samples in liquid environment: wepresent here a study about AFM imaging of living, moving or self-immobilized bacteria, in their genuine physiological liquid medium and in true in vivo conditions. No external immobilization protocol, neither chemical nor mechanical was needed. For the first time, the native gliding movements of Gram negative Nostoc cyanobacteria upon the surface were studied by AFM. AFM height and mechanical stiffness data were simultaneously acquired. From these, mechanical parameters, inner turgor pressure and Young modulus, were derived for different bacterial species (Anabaenopsis circularis, Rhodococcus wratislaviensis). Our study revealed that AFM imaging is thus possible on moving living species. These results open a large window on new studies of both dynamical phenomena of practical and fundamental interests such as the formation of biofilms and dynamic properties of bacteria in real physiological conditions. The second delicate step was to combine AFM and optical measurements with electrical ones. We mounted a new experimental set-up coupling real-time (i) monitoring of optical properties as the optical density (OD) evolution related to bulk bacterial growth in liquid or as the counting of number of bacteria adhering on the surface of the sample as well and (ii) electrical and electrochemical measurements. Furthermore, these results will shortly be applied to the optimized monitoring of the in-situ activity of bacteria consuming oil pollutants, following this way, in real-time, the bioremediation of an oilcontaminated soil (ANR ECOTECH_BIOPHY program).
La présence de matière biologique (biofilms) dans les sites de stockage géologique profond, d'éléments toxiques ou encore de l'eau potable des aquifères est maintenant clairement démontrée. Cette biomasse est à l'origine de processus physiques et chimiques qui modifient considérablement la durabilité et la pérennité des sites concernés. Ces processus, principalement de type oxydo-réductif, sont encore mal compris. Ceci est principalement dû aux méthodes d'investigation, principalement macroscopiques, loin de l'échelle micrométrique caractéristique des bactéries. Seules des études, basées sur des méthodes d'investigation locale, peuvent apporter les informations requises. Ainsi, nous avons développé un dispositif expérimental basé sur l'utilisation combinée de la microscopie optique (en transmission), la microscopie à force atomique (AFM) et la microscopie AFM en mode électrique et électrochimique (EC_AFM) afin d'obtenir des informations simultanées sur la topographie de l'échantillon et sur les processus électrochimiques à l'échelle des bactéries. La première étape sensible consistait à utiliser l'AFM sur des échantillons biologiques en milieu liquide: nous présentons ici les résultats de l'imagerie AFM en milieu liquide de plusieurs types de bactéries dans leurs conditions physiologiques naturelles (conditions in vivo). Aucun protocole d'immobilisation, ni chimique ni mécanique, n'a été nécessaire; et pour la première fois, les mouvements de reptation de cyanobactéries Nostoc ont été étudiés par l'AFM. Les études AFM ont permis d'acquérir des données topographiques mais aussi mécaniques : nous avons pu ainsi mesurer le module d'Young, la pression de turgescence de différentes souches bactériennes (Anabaenopsis circularis, Rhodococcus wratislaviensis). Cette étude complète, a révélé que l'imagerie AFM est donc possible sur des espèces vivantes en mouvement. Ces résultats ouvrent une grande fenêtre sur de nouvelles études d'intérêts tels que la formation de biofilms et les propriétés dynamiques de bactéries dans des conditions physiologiques réelles. La deuxième étape délicate était de combiner l'AFM aux mesures optiques et électriques. Nous avons développé un nouveau dispositif expérimental permettant (i) le suivi de l'évolution de la croissance bactérienne par la mesure des propriétés optiques comme la densité optique DO (pour le développement bactérien en volume - milieu planctonique) , ou l'analyse de l'image du substrat par comptage du nombre de bactéries sur la surface de l'échantillon (biofilm), et (ii) les mesures électriques et électrochimiques. L'ensemble de ces résultats sera prochainement appliqué au développement de nouveaux outils de surveillance d'une biodépollution de terrain contaminé par les hydrocarbures, par le suivi in situ et en temps réel de l'activité de bactéries dépolluantes (ECOTECH_BIOPHY ANR).
https://tel.archives-ouvertes.fr/tel-01044714

tel-01044714
https://tel.archives-ouvertes.fr/tel-01044714
https://tel.archives-ouvertes.fr/tel-01044714/document
https://tel.archives-ouvertes.fr/tel-01044714/file/theseDhahri2013.pdf

Éditeur(s) : HAL CCSD Elsevier
Résumé : International audience
Properties of composite materials depend on interatomic phenomena occurring between binder crystals. Experimental information of Atomic Force Microscopy (A.F.M.) is of prime importance; however understanding is helped by molecular modeling. As underlined in Section 1, the present study is able to simulate crystal interfaces in presence of a solution within apertures less than 1 Nanometer at a full atomic scale. Section 2 presents the case study of a gypsum solution between (120) gypsum faces, with related boundary conditions and atomic interactions. Section 3 deals with the mass equilibrium of the solution within interfaces <5 angstrom, using the original Semi Analytical Stochastic Perturbations (SASP) approach. This information becomes in Section 4 the key for explaining the peak of adhesion obtained in A.F.M. around an aperture of 3 A and gives enlightenments on gypsum cohesion. In conclusion, this illustration shows the potentialities of full atomic modeling which could not be attained by any numerical approach at a mesoscopic scale.
ISSN: 0008-8846

hal-00411868
https://hal.archives-ouvertes.fr/hal-00411868
DOI : 10.1016/j.cemconres.2007.09.022

Éditeur(s) : HAL CCSD American Physical Society
Résumé : We study the equilibrium properties of a liquid phase condensed at the nanoscale between the surfaces of a sharp crack in fused silica in a moist controlled atmosphere. The extension of the condensed phase along the fracture is measured by in situ atomic force microscopy phase imaging and it is shown to be determined by a critical distance between the opposite crack surfaces, which is an increasing function of humidity. The present technique is very promising for measuring the properties of confined liquids at the nanoscale as well as for modeling the physics and chemistry of slow crack propagation in glasses.
ISSN: 0031-9007

hal-00411946
https://hal.archives-ouvertes.fr/hal-00411946
DOI : 10.1103/PhysRevLett.100.165505

Éditeur(s) : HAL CCSD Elsevier
Résumé : International audience
GenMol (TM) code is used to simulate Atomic Force Microscopy (AFM) tests at a kaolinite/brine/kaolinite contact, the confined fluid in sub-nanometre interspaces being in equilibrium with an external multi-species solution. The attraction/repulsion effort, i.e. the derivative versus the interspace aperture h of the interaction energy between both kaolinite faces, is computed versus the variable composition of the confined fluid (see for the method Part I of this work). Two external solutions are tested. Solution Si is a neutral brine (pH=7.5) leading to a possible attraction for apertures lower than 7 angstrom. Solution S2 is an acidified brine (pH=3.2) leading to repulsion whatever may be the aperture h. These two AFM simulations prove the existence of a critical pH value (3.2 < pH(crit) < 7.5) of the external solution, below which the acidification of a natural brine in a CO2 confinement inhibits adhesion between kaolinite aggregates.
ISSN: 0022-0248

hal-00544678
https://hal.archives-ouvertes.fr/hal-00544678
DOI : 10.1016/j.jcrysgro.2010.08.012

Éditeur(s) : HAL CCSD Springer Verlag
Résumé : International audience
Nanotribological properties of NbSe2 are studied using an atomic friction force microscope. The friction force is measured as a function of normal load and scan speeds ranging from 10 nm s−1 to 40 μm s−1 under two atmospheres (air and argon). At low speed, no effect of atmosphere is noticed and a linear relationship between the friction and normal forces is observed leading to a friction coefficient close to 0.02 for both atmospheres. At high speed, the tip/surface contact obeys the JKR theory and the tribological properties are atmosphere dependent: the shear stress measured in air environment is three times lower than the one measured under argon atmosphere. A special attention is paid to interpret these results through numerical data obtained from a simple athermal model based on Tomlinson approach.
ISSN: 1023-8883

hal-00780496
https://hal.archives-ouvertes.fr/hal-00780496
https://hal.archives-ouvertes.fr/hal-00780496/document
https://hal.archives-ouvertes.fr/hal-00780496/file/Delbe_6345.pdf
DOI : 10.1007/s11249-008-9400-8

Éditeur(s) : HAL CCSD wiley
Résumé : International audience
The slow advance of a crack in sodo-silicate glasses was studied at nanometer scale by in-situ atomic force microscopy (AFM) in a well-controlled atmosphere (N2 and H2O). An enhanced diffusion of sodium ions in the stress-gradient field at the sub-micrometric vicinity of the crack tip was revealed through several effects: growth of nodules in height images, changes in the AFM tip–sample energy dissipation as detected in phase images. Ex-situ chemical micro-analyses completed the AFM measurements. The nodules patterns revealed a dewetting phenomenon evidenced by “breath figures”, i.e. analog to the fogging that occurs when a vapour condenses onto a 'cold' surface [D. Beysens et al., Phys. Rev. Let. 57, 1433 (1986)]. These experimental results were explained by a two-step process: i) a fast migration of sodium ions towards the fracture surfaces as proposed by Langford et al. [J. Mat. Res. 6, 1358 (1991)], ii) a slow backwards diffusion of the cations as evidenced in these AFM experiments (typical time: few minutes). Measurements of the diffusion coefficient of that relaxing process were done at room temperature. Our results strengthen the theoretical concept of a near-surface structural relaxation due to the stress-gradient at the vicinity of the crack tip. Raman and SIMS studies revealed that nodules – for samples studied after exposition to common air - are preferentially covered by an organic overlayer of a carboxylate salt with a long aliphatic chain. The catalytic role of sodium ions in that chemical process is suspected.
Fractography of glasses an ceramics V
Rochester, United States

hal-00408605
https://hal.archives-ouvertes.fr/hal-00408605

Éditeur(s) : HAL CCSD Elsevier
Résumé : International audience
Porous thin films considered for applications like separation, sensing and microelectronic have to sustain mechanical stresses during their integration process or in working conditions. Thanks to recent progress in processing methods, it is now possible to precisely control the porosity and combine ordered mesopores with randomly-distributed macropores to achieve hierarchically porous materials. The mechanical properties of thin films containing different types of porosity (ordered meso, random macro and hierarchical) have been investigated by means of nanoindentation. In particular a method recently proposed by Li and Vlassak (H. Li, J.J. Vlassak, Journal of Materials Research 24 (2009) 1114-1126) is applied to account for the substrate effect. Residual indent impressions were imaged by Atomic Force Microscopy (AFM) to provide some insights in the mechanical behavior of the films. In addition, experimental indentation moduli are compared to theoretical predictions obtained via Finite Element (FE) analysis. The different porous structures have been modeled by FE to obtain the effective elastic properties from which the indentation modulus can be inferred. Finally, the experimental-model differences are discussed. © 2010 Elsevier Inc. All rights reserved.
ISSN: 1387-1811

hal-01683194
https://hal.univ-antilles.fr/hal-01683194
DOI : 10.1016/j.micromeso.2010.09.004

Éditeur(s) : HAL CCSD Public Library of Science
Résumé : 51 pages; 15figures; 3 tables, accepted for publication in PloS ONE
International audience
We present a study about AFM imaging of living, moving or self-immobilized, bacteria in their genuine physiological liquid medium. No external immobilization protocol, neither chemical nor mechanical, was needed. For the first time, the native gliding movements of Gram-negative Nostoc cyanobacteria upon the surface, at speeds up to 900microns/h, were studied by AFM. This was possible thanks to an improved combination of a gentle sample preparation process and an AFM procedure based on fast and complete force-distance curves made at every pixel, drastically reducing lateral forces. No limitation in spatial resolution or imaging rate was detected. Gram-positive and non-motile R. wratislaviensis bacteria were studied as well. From the approach curves, Young modulus and turgor pressure were measured for both strains at different gliding speeds and are ranging from 20±3 to 105±5MPa and 40±5 to 310±30kPa depending on the bacterium and the gliding speed. For Nostoc, spatially limited zones with higher values of stiffness were observed. The related spatial period is much higher than the mean length of Nostoc nodules. This was explained by an inhomogeneous mechanical activation of nodules in the Nostoc. We also observed the presence of a soft extra cellular matrix (ECM) around the Nostoc. Both strains left a track of polymeric slime with variable thicknesses. For R. wratislaviensis, it is equal to few hundreds of nanometers, likely to promote its adhesion to the sample. While gliding, the Nostoc secretes a slime layer the thickness of which is in the nanometer range and increases with the gliding speed.
ISSN: 1932-6203

hal-00769765
https://hal.archives-ouvertes.fr/hal-00769765
https://hal.archives-ouvertes.fr/hal-00769765v3/document
https://hal.archives-ouvertes.fr/hal-00769765/file/REsubmission_In-situ_determination_Dhahri_Plos_One_R2_Hal.pdf

Éditeur(s) : HAL CCSD Wiley
Résumé : 13 pages, 4 figures, to be published on J. Am. Cer. Soc
International audience
Since crack propagation in oxide materials at low crack velocities is partly determined by chemical corrosion, proper knowledge of the crack tip chemistry is crucial for understanding fracture in these materials. Such knowledge can be obtained only from in situ studies because the processes that occur in the highly confined environment of the crack tip are very different from those that take place at free surfaces, or that can be traced post mortem. We report the occurrence of hydrous liquid condensate between the two fracture surfaces in the vicinity of the tip of tensile cracks in silica. Observations are performed in real-time by means of atomic force microscopy (AFM) at continuously controlled crack velocities in the regime of stress corrosion. Condensate formation and changes in extent and shape are demonstrated for a wide range of macroscopic humidity at different crack speeds. Its liquid character is confirmed by the study of AFM phase-contrast data. It is believed that this evidence of a nanoscale liquid hydrous phase at the crack tip will enable novel insights in the chemistry of failure of oxide materials.
ISSN: 0002-7820

hal-00424984
https://hal.archives-ouvertes.fr/hal-00424984
ARXIV : cond-mat/0509209
DOI : 10.1111/j.1551-2916.2005.00765.x

Éditeur(s) : HAL CCSD Elsevier
Résumé : The slow advance of a crack in soda-silicate glasses was studied at nanometer scale by in-situ and real-time atomic force microscopy (AFM) in a well-controlled atmosphere. An enhanced diffusion of sodium ions in the stress-gradient field at the sub-micrometric vicinity of the crack tip was revealed through several effects: growth of nodules in AFM height images, changes in the AFM tip–sample energy dissipation. The nodules patterns revealed a dewetting phenomenon evidenced by ‘breath figures'. Complementary chemical micro-analyses were done. These experimental results were explained by a two-step process: (i) a fast migration (typical time: few milliseconds) of sodium ions towards the fracture surfaces as proposed by Langford et al. [J. Mat. Res. 6 (1991) 1358], (ii) a slow backwards diffusion of the cations as evidenced in these AFM experiments (typical time: few minutes). Measurements of the diffusion coefficient of that relaxing process were done at room temperature. Our results strengthen the theoretical concept of a near-surface structural relaxation due to the stress-gradient at the vicinity of the crack tip. The inhomogeneous migration of sodium ions might be a direct experimental evidence of the presence of sodium-rich channels in the silicate structure [A. Meyer et al., Phys. Rev. Let. 93 (2004) 027801].
ISSN: 0022-3093

hal-00407634
https://hal.archives-ouvertes.fr/hal-00407634
DOI : 10.1016/j.jnoncrysol.2006.09.034

Éditeur(s) : HAL CCSD American Institute of Physics
Résumé : International audience
Laser-induced periodic surface structures (LIPSS) were formed on Cu/Si or Cu/glass thin films using Nd:YAG laser beam (40 ps, 10Hz, and 30mJ/cm2). The study of ablation threshold is always achieved over melting when the variation of the number of pulses increases from 1 to 1000. But the incubation effect is leading to reduce the threshold of melting as increasing the number of laser pulse. Also, real time reflectivity signals exhibit typical behavior to stress the formation of a liquid phase during the laser-processing regime and helps to determine the threshold of soft ablation.Atomic Force Microscopy (AFM) analyses have shown the topology of the micro-crater containing regular spikes with different height. Transmission Electron Microscopy (TEM) allows finally to show three distinguished zones in the close region of isolated protrusions. The central zone is a typical crystallized area of few nanometers surrounded by a mixed poly-crystalline and amorphous area. Finally, in the region far from the protrusion zone, Cu film shows an amorphous structure. The real time reflectivity, AFM, and HR-TEM analyses evidence the formation of a liquid phaseduring the LIPSS formation in the picosecond regime. VC 2015 AIP Publishing LLC
ISSN: 0003-6951

hal-01226065
https://hal.archives-ouvertes.fr/hal-01226065
DOI : 10.1063/1.4935413

Éditeur(s) : HAL CCSD Elsevier
Résumé : Water molecules play a fundamental role in the physics of slow crack propagation in glasses. It is commonly understood that, during stress-corrosion, water molecules that move in the crack cavity effectively reduce the bond strength at the strained crack tip and, thus, support crack propagation. Yet the details of the environmental condition at the crack tip in moist air are not well determined. In a previous work, we reported direct evidence of the presence of a 100 nm long liquid condensate at the crack tip in fused silica glass during very slow crack propagation (10(-9)-10(-10) m/s). These observations are based on in situ AFM phase imaging techniques applied on DCDC glass specimens in controlled atmosphere. Here, we discuss the physical origin of the AFM phase contrast between the liquid condensate and the glass surface in relation to tip-sample adhesion induced by capillary bridges. We then report new experimental data on the water condensation length increase with relative humidity in the atmosphere. The measured condensation lengths were much larger than what predicted using the Kelvin equation and expected geometry of the crack tip.
ISSN: 0022-3093

hal-00412153
https://hal.archives-ouvertes.fr/hal-00412153
DOI : 10.1016/j.jnoncrysol.2007.06.090

Éditeur(s) : HAL CCSD
Résumé : International audience
A key element of the biomechanical design of trees is their ability to generate largemechanical stresses in wood at the stem periphery. This function is necessary for the tree tocontrol the orientation of its axes, and therefore to grow in height, maintain its branches at anoptimal angle or achieve adaptive reorientations (Fournier et al., 2013). This “maturationstress” appears in wood fibres during their cellular maturation when their secondary cell wallis thickening. In hardwoods, the stress asymmetry is generated by the formation of specificfibres with a very high tensile growth stress on the upper side of the inclined axis. Theresulting tension wood has microstructural features highly different from the normal wood.Tension wood in almost all temperate species has a specific gelatinous cell wall layer, calledG-layer, that is not lignified and highly mesoporous (Chang et al., 2015). It has been shownrecently, at the macroscopic scale, that cellulose tension appears during maturation and issynchronous with the development of this specific layer (Clair et al., 2011). Tropical species,like simarouba, are able to generate lignified tension wood fibres. The mechanisms of stressgeneration in tension wood fibres are not yet well known. The aim of our study is tounderstand these mechanisms and to know the spatial and temporal kinetics of the differentcell wall layers stiffening during maturation, in parallel with tensile stress generation.Contact-Resonance Atomic Force Microscopy, CR-AFM, was used here to address thisquestion on embedded samples (Arnould and Arinero, 2015) using dual resonance frequencytracking (DRFT, Rodriguez et al., 2007). Change in the contact modulus between, and within,each layer of the cell wall has been measured on several radial lines of developing fibres atdifferent steps. In order to understand the obtained results, and to estimate the sensitivity ofthe AFM indentation-like technique to the different cell wall components stiffness, an elasticanisotropic indentation model was used (Vlassak et al., 2003; Jäger et al., 2011). Finally,these mechanical measurements have been compared to topochemical data obtained on thesame fibres.
8th Plant Biomechanics International Conference
Nagoya, Japan

hal-01436113
https://hal.archives-ouvertes.fr/hal-01436113