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Manfred May

Publications and source records attributed to Manfred May.

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Directional Dark Field for Nanoscale Full-Field Transmission X-Ray Microscopy

Dark-field X-ray imaging visualizes structural inhomogeneities through small-angle scattering, but existing directional methods are confined to the micrometer scale. While recent advances have extended dark-field capabilities to nanoscale transmission X-ray microscopy, directional scattering retrieval - critical for characterizing anisotropic nanostructures - has remained inaccessible for imaging resolutions in the sub-micrometer scale. Here, we demonstrate the first directional dark-field setup for nanoimaging, achieving orientation mapping of scattering features below the spatial resolution limit. Our method is experimentally simple to implement with existing transmission X-ray microscopy setups. We validate its performance by successfully resolving sub-resolution test structure orientations, cross-correlating orientational changes within hierarchical nanoporous materials, and mapping the directional arrangement of hydroxyapatite nanocrystals 30 - 70 nm within human tooth enamel. By utilizing shadow regions in the optical configuration, we further extend the detectable scattering vector range, demonstrating a pathway toward size-selective dark-field imaging. This advancement enables the quantitative structural characterization of anisotropic nanomaterials, which are critical to biomineralization, advanced materials, and nanotechnology applications.

physics.optics

Wafer-scale fabrication of mesoporous silicon functionalized with electrically conductive polymers

The fabrication of hybrid materials consisting of nanoporous hosts with conductive polymers is a challenging task, since the extreme spatial confinement often conflicts with the stringent physico-chemical requirements for polymerization of organic constituents. Here, several low-threshold and scalable synthesis routes for such hybrids are presented. First, the electrochemical synthesis of composites based on mesoporous silicon (pore size of 7 nm) and the polymers PANI, PPy and PEDOT is discussed and validated by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). Polymer filling degrees of 74% are achieved. Second, the production of PEDOT/pSi hybrids, based on the solid-state polymerization (SSP) of DBEDOT to PEDOT is shown. The resulting amorphous structure of the nanopore-embedded PEDOT is investigated via in-situ synchrotron-based X-ray scattering. In addition, a twofold increase in the electrical conductivity of the hybrid compared to the porous silicon host is shown, making this system particularly promising for thermoelectric applications.

cond-mat.mtrl-sci

How nanoporous silicon-polypyrrole hybrids flex their muscles in aqueous electrolytes: In operando high-resolution x-ray diffraction and electron tomography-based micromechanical computer simulations

Macroscopic strain experiments revealed that Si crystals traversed by parallel, channel-like nanopores functionalized with the muscle polymer polypyrrole exhibit large and reversible electrochemo-mechanical actuation in aqueous electrolytes. On the microscopical level this system still bears open questions, as to how the electrochemical expansion and contraction of PPy acts on to np-Si pore walls and how the collective motorics of the pore array emerges from the single-nanopore behavior. An analysis of in operando X-ray diffraction experiments with micromechanical finite element simulations, based on a 3D reconstruction of the nanoporous medium by TEM tomography, shows that the in-plane mechanical response is dominantly isotropic despite the anisotropic elasticity of the single crystalline host matrix. However, the structural anisotropy originating from the parallel alignment of the nanopores lead to significant differences between the in- and out-of-plane electromechanical response. This response is not describable by a simple 2D arrangement of parallel cylindrical channels. Rather, the simulations highlight that the dendritic shape of the Si pore walls, including pore connections between the main channels, cause complex, inhomogeneous stress-strain fields in the crystalline host. Time-dependent X-ray scattering on the dynamics of the actuator properties hint towards the importance of diffusion limitations, plastic deformation and creep in the nanoconfined polymer upon (counter-)ion adsorption and desorption, the very pore-scale processes causing the macroscopic electroactuation. From a more general perspective, our study demonstrates that the combination of TEM tomography-based micromechanical modeling with high-resolution X-ray scattering experiments provides a powerful approach for in operando analysis of nanoporous composites from the single-nanopore up to the porous-medium scale.

cond-mat.mtrl-sci