Quantitative AFM analysis of phase separated borosilicate glass surfaces

Dalmas, Davy; Lelarge, Anne; Vandembroucq, Damien

doi:10.1016/j.jnoncrysol.2007.07.005

Cited by 15 publications

(20 citation statements)

References 27 publications

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“…A fast quench below the glass transition temperature enables one to study the frozen structure in the solid state, thereby extending the variety of available characterization techniques. Transmission and scanning electron microscopy, Raman Scattering and Atomic Force Microscopy have been used to characterize quantitatively phase separation in glasses [27][28][29]. We focus here on the late stage of spinodal decomposition after a deep quench into the unstable region, that produces interconnected structures.…”

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confidence: 99%

Fragmentation and Limits to Dynamical Scaling in Viscous Coarsening: An Interruptedin situX-Ray Tomographic Study

et al. 2014

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X-Ray microtomography was used to follow the coarsening of the structure of a ternary silicate glass experiencing phase separation in the liquid state. The volumes, surfaces, mean and Gaussian curvatures of the domains of minority phase were measured after reconstruction of the 3D images and segmentation. A linear growth law of the characteristic length scale ∼ t was observed. A detailed morphological study was performed. While dynamical scaling holds for most of the geometrical observables under study, a progressive departure from scaling invariance of the distributions of local curvatures was evidenced. The latter results from a gradual fragmentation of the structure in the less viscous phase that also leads to a power-law size distribution of isolated domains.Introduction -The construction of a theoretical framework describing the phase separation of binary liquids [1][2][3] has been fueled by successive experimental developments. Up to the 90's, most experimental observations were performed in the Fourier space, with light or neutron scattering. Model systems were immiscible solutions [4,5], and polymer blends [6,7], or glasses [8]. These experiments confirmed that the dynamical scaling assumption is relevant for these systems, i.e. it is possible to rescale the structure factor by a unique length scale . This length increases with a power law: (t) ∼ t α , α depending on the growth regime [9]. More recent numerical simulations confirmed this scaling behavior, and provided some insights about the geometry in real space [10][11][12]. Meanwhile, access to direct space was made possible by new techniques of observation, such as scanning laser confocal microscopy: curvatures could be measured on phase-separated polymer blends [13,14]. These observations are especially relevant to discuss the local mechanisms that govern the coarsening: pinch-off was for instance observed in a colloidal glass [15]. Recent predictions concerning statistical quantities such as size or surface distributions of domains [16,17] and numerical studies of aging in phase-separating fluids [18,19] also motivate the observation in real space.The effect of the mobility on the morphology has recently raised a growing interest. Experiments on polymers revealed the spectacular influence of visco-elasticity [20]. Recent work [21] evidenced a logarithmic (stressassisted) growth for a gas-glass phase separation. Numerical simulations with a viscosity contrast [22,23] showed a strong effect on morphology. However, the influence of a sole viscosity contrast has not yet been experimentally investigated in the hydrodynamical regime.The development of X-ray microtomography provides an suitable tool to explore phase separation in 3-D, with submicron spatial resolution reached in Synchrotron facilities [24,25]. Phase-separated polymer blends were

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confidence: 99%

Fragmentation and Limits to Dynamical Scaling in Viscous Coarsening: An Interruptedin situX-Ray Tomographic Study

et al. 2014

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“…for each thermal treatment conditions), at least 3 AFM images were performed for 4 different scan areas ranging between 500 × 500 nm 2 and 8 × 8 µm 2 .Beyond its imaging ability, AFM has recently been used as a truly quantitative tool to study glass surfaces. It is, for example, possible to obtain a quantitative validation of the description of fused glass surfaces by frozen capillary waves [21] or of the kinetics of phase separation in glasses [20]. In both cases, not only are the expected scaling regimes recovered but the prefactors of the scaling laws can also be extracted and shown to be consistent with the associated physical parameters (diffusivity, interface tension).…”

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“…Even in the simpler case of plane crack propagation, the roughness exponent characterising the in-plane roughness of the crack front was found to be significantly lower in models (ζ dep H ≃ 0.4) [18,19] than in experiments (ζ H ≃ 0.55) [8].We argue here within that the main reason for the apparent discrepancy between experimental results and scaling predictions of depinning models stems from the dubious status in most experiments of a key hypothesis of the models: a clear separation between the scale of disorder and the scale of measurement. To test this argument, we present results of fracture experiments performed on a series of model heterogeneous brittle materials: phase separated glasses [20]. Thermal treatments of various durations allowed the fine tuning of phase domain sizes.…”

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confidence: 99%

“…Further details concerning the preparation and the characterisation of the glass samples can be found in Ref. [20].Stable dynamic fracture experiments on these heterogeneous materials were performed by using a DCDC set-up (Double Cleavage Drilled Compression) (see Fig. 1-Left) and a statistical analysis of the fracture surface roughness carried out from Atomic Force Microscopy (AFM) images (see Fig.…”

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Crack Propagation through Phase-Separated Glasses: Effect of the Characteristic Size of Disorder

2008

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We perform fracture experiments on nanoscale phase-separated glasses and measure crack surface roughness by atomic force microscopy. The ability of tuning the phase domain size by thermal treatment allows us to test thoroughly the predictions of crack front depinning models about the scaling properties of crack surface roughness. It appears that, in the range of validity of these depinning models developed for the fracture of brittle materials, our experimental results show a quantitative agreement with theoretical predictions: Beyond the characteristic size of disorder, the roughness of crack surfaces obeys the logarithmic scaling early predicted by Ramanathan, Ertaş, and Fisher [Phys. Rev. Lett. 79, 873 (1997)].

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“…New insights on phase separation paralleled the emergence of experimental techniques in materials science. Whereas the first kinetic studies were realized in the Fourier space, using light diffusion techniques [31,1], direct access to the morphology of the phases is now possible thanks to imaging techniques such as electronic microscopy [32], atomic force microscopy [21,20], X-ray tomography [33] or atom probe tomography [34,23]. In-situ synchrotron microtomography [35] is a technique of choice for studying microstructure formation [36,37], since it provides both the 3-D microstructure and its topology, and successive snapshots of its evolution.…”

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confidence: 99%

Hydrodynamic coarsening in phase-separated silicate melts

et al. 2015

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Using in-situ synchrotron tomography, we investigate the coarsening dynamics of barium borosilicate melts during phase separation. The 3-D geometry of the two interconnected phases is determined thanks to image processing. We observe a linear growth of the size of domains with time, at odds with the sublinear diffusive growth usually observed in phase-separating glasses or alloys. Such linear coarsening is attributed to viscous flow inside the bicontinuous phases, and quantitative measurements show that the growth rate is well explained by the ratio of surface tension over viscosity. The geometry of the domains is shown to be statistically similar at different times, provided that the microstructure is rescaled by the average domain size. Complementary experiments on melts with a droplet morphology demonstrate that viscous flow prevails over diffusion in the large range of domain sizes measured in our experiments (1 -80 µm).

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Quantitative AFM analysis of phase separated borosilicate glass surfaces

Cited by 15 publications

References 27 publications

Fragmentation and Limits to Dynamical Scaling in Viscous Coarsening: An Interruptedin situX-Ray Tomographic Study

Fragmentation and Limits to Dynamical Scaling in Viscous Coarsening: An Interruptedin situX-Ray Tomographic Study

Crack Propagation through Phase-Separated Glasses: Effect of the Characteristic Size of Disorder

Hydrodynamic coarsening in phase-separated silicate melts

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