SummaryThree-dimensional (3D) data represent the basis for reliable quantification of complex microstructures. Therefore, the development of high-resolution tomography techniques is of major importance for many materials science disciplines. In this paper, we present a novel serial sectioning procedure for 3D analysis using a dual-beam FIB (focused ion beam). A very narrow and reproducible spacing between the individual imaging planes is achieved by using drift correction algorithms in the automated slicing procedure. The spacing between the planes is nearly of the same magnitude as the pixel resolution on scanning electron microscopy images. Consequently, the acquired stack of images can be transformed directly into a 3D data volume with a voxel resolution of 6 × 7 × 17 nm. To demonstrate the capabilities of FIB nanotomography, a BaTiO 3 ceramic with a high volume fraction of fine porosity was investigated using the method as a basis for computational microstructure analysis and the results compared with conventional physical measurements. Significant differences between the particle size distributions as measured by nanotomography and laser granulometry indicate that the latter analysis is skewed by particle agglomeration/aggregation in the raw powder and by uncertainties related to calculation assumptions. Significant differences are also observed between the results from mercury intrusion porosimetry (MIP) and 3D pore space analysis. There is strong evidence that the ink-bottle effect leads to an overestimation of the frequency of small pores in MIP. FIB nanotomography thus reveals quantitative information of structural features smaller than 100 nm in size which cannot be acquired easily by other methods.

Targeting of immunoglobulin E (IgE) represents an interesting approach for the treatment of allergic disorders. A high-affinity monoclonal anti-IgE antibody, ligelizumab, has recently been developed to overcome some of the limitations associated with the clinical use of the therapeutic anti-IgE antibody, omalizumab. Here, we determine the molecular binding profile and functional modes-of-action of ligelizumab. We solve the crystal structure of ligelizumab bound to IgE, and report epitope differences between ligelizumab and omalizumab that contribute to their qualitatively distinct IgE-receptor inhibition profiles. While ligelizumab shows superior inhibition of IgE binding to FcεRI, basophil activation, IgE production by B cells and passive systemic anaphylaxis in an in vivo mouse model, ligelizumab is less potent in inhibiting IgE:CD23 interactions than omalizumab. Our data thus provide a structural and mechanistic foundation for understanding the efficient suppression of FcεRI-dependent allergic reactions by ligelizumab in vitro as well as in vivo.

The aim of the present investigation is to define microstructure parameters, which control the effective transport properties in porous materials for energy technology. Recent improvements in 3D-imaging (FIB-nanotomography, synchrotron X-ray tomography) and image analysis (skeletonization and graph analysis, transport simulations) open new possibilities for the study of microstructure effects. In this study, we describe novel procedures for a quantitative analysis of constrictivity, which characterizes the so-called bottleneck effect. In a first experimental part, methodological tests are performed using a porous (La,Sr)CoO 3 material (SOFC cathode). The tests indicate that the proposed procedure for quantitative analysis of constrictivity gives reproducible results even for samples with inhomogeneous microstructures (cracks, gradient of porosity). In the second part, 3D analyses are combined with measurements of ionic conductivity by impedance spectroscopy. The investigations are preformed on membranes of electrolysis cells with porosities between 0.27 and 0.8. Surprisingly, the tortuosities remain nearly constant (1.6) for the entire range of porosity. In contrast, the constrictivities vary strongly and correlate well with the measured transport resistances. Hence, constrictivity represents the dominant microstructure parameter, which controls the effective transport properties in the analysed membrane materials. An empirical relationship is then derived for the calculation of effective transport properties based on phase volume fraction, tortuosity, and constrictivity.

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[1] Local porosity theory in combination with percolation theory was applied to shale microstructures that were reconstructed on the basis of focused ion beam nanotomography and scanning transmission electron microscopy. This allowed characterizing pore microstructures in Opalinus clay with length scales on the order of tens of microns. In a sample from the sandy facies (with low clay content), the fraction of "larger" pores f(radii~> 15 nm) = 0.076 is substantially higher than that in the shaley facies (with a higher clay content), where f(radii~> 15 nm) = 0.015. The resolved porosity possesses a certain degree of homogeneity, and the representative volume element (RVE) of porosity can be determined in terms of a given relative error on porosity. For example, if we accept a relative error of 10%, the RVE is on the scale of a few hundreds of microns. Both pore microstructures from sandy and shaley facies show anisotropic characteristics with respect to connectivity and percolation threshold. Using finite scaling, we found percolation thresholds with critical porosities f c,b = 0.04-0.12 parallel to bedding and f c,perp = 0.11-0.19 perpendicular to bedding. The resolved porosity of the sandy facies (low clay content) is close to the percolation threshold, whereas the porosity of the shaley facies (high clay content) is below the percolation threshold. The porosity in carbonate layers is around f = 0.027, and the pore size is substantially larger when compared to the pores in the clay matrix. In the analyzed sample, pores in carbonate layers are poorly connected.Citation: Keller, L. M., L. Holzer, P. Schuetz, and P. Gasser (2013), Pore space relevant for gas permeability in Opalinus clay: Statistical analysis of homogeneity, percolation and representative volume element,

A new 3D-microscopy method, focused ion beam-nanotomography (FIB-nt), has been applied to the statistical particle shape analysis and for topological characterization of granular textures in cement samples. Because of its high resolution (15 nm), FIB-nt reveals precise microstructural information at the submicrometer scale, which cannot be obtained with conventional tomography methods. It is demonstrated that even from complex granular textures with dense agglomerates, it is possible to identify the individual sub-grains. This is the basis for reliable statistical shape analysis. For this purpose, moments of inertia were determined for particles from five different grain size fractions of a given cement, which provides important input data for future modeling of rheology and hydration processes. In addition, FIB-nt was used for topological characterization of the particle-particle interfaces in the dense and fine-grained granular textures. The unique 3D-data obtained with FIB-nt thus open new possibilities for quantitative microstructure analysis and the data can be used as structural input for object-oriented modeling.

The focused ion beam‐nanotomography (FIB‐nt) technique presented in Part I of this article is a novel high‐resolution three‐dimensional (3D) microscopy method that opens new possibilities for the microstructural investigation of fine‐grained granular materials. Specifically, FIB‐nt data volumes allow particle size distributions (PSD) to be determined, and the current paper discusses all the processing steps required to obtain the PSD from 3D data. This includes particle recognition and the subsequent PSD estimation. A refined watershed approach for 3D particle recognition that tolerates concavities on the particle surfaces is presented. Particles at the edge of the 3D data volume are invariably clipped, and because the data volume is of a very limited size, this effect of boundary truncation seriously affects the PSD and needs to be corrected. Therefore, two basic approaches for the stereological correction of the truncation effects are proposed and validated on artificially modeled particle data. Finally, the suggested techniques are applied to real 3D‐particle data from ordinary portland cement and the resulting PSDs compared with data from laser granulometry.