The successfuls ynthesis of hierarchically structured titaniums ilicalite-1 (TS-1) with large intracrystalline macroporesb ys team-assisted crystallisation of mesoporous silica particlesi sr eported. The macropore topologyw as imaged in 3D by using electron tomographya nd synchrotron radiation-based ptychographic X-ray computed tomography,r evealing interconnected macropores within the crystals accounting for about3 0% of the particle volume. The study of the macropore formation mechanism revealed that the mesoporous silica particles act as as acrificial macropore template during the synthesis. Silicon-to-titanium ratio of the macroporous TS-1 samples was successfully tuned from 100 to 44. The hierarchically structured TS-1 exhibited high activity in the liquid phase epoxidation of 2-octene with hydrogen peroxide.T he hierarchically structured TS-1 surpassed ac onventional nano-sized TS-1 sample in terms of alkene conversion and showed comparable selectivity to the epoxide. The flexible synthesis route described herec an be used to prepare hierarchical zeolites with improved mass transport properties for other selective oxidation reactions.

The NanoMAX hard X-ray nanoprobe is the first beamline to take full advantage of the diffraction-limited storage ring at the MAX IV synchrotron and delivers a high coherent photon flux for applications in diffraction and imaging. Here, we characterize its coherent and focused beam using ptychographic analysis. We derive beam profiles in the energy range 6-22 keV and estimate the coherent flux based on a probe mode decomposition approach.

NanoMAX is the first hard X-ray nanoprobe beamline at the MAX IV laboratory. It utilizes the unique properties of the world's first operational multi-bend achromat storage ring to provide an intense and coherent focused beam for experiments with several methods. In this paper we present the beamline optics design in detail, show the performance figures, and give an overview of the surrounding infrastructure and the operational diffraction endstation.

This paper presents a deep learning algorithm for tomographic reconstruction (GANrec). The algorithm uses a generative adversarial network (GAN) to solve the inverse of the Radon transform directly. It works for independent sinograms without additional training steps. The GAN has been developed to fit the input sinogram with the model sinogram generated from the predicted reconstruction. Good quality reconstructions can be obtained during the minimization of the fitting errors. The reconstruction is a self‐training procedure based on the physics model, instead of on training data. The algorithm showed significant improvements in the reconstruction accuracy, especially for missing‐wedge tomography acquired at less than 180° rotational range. It was also validated by reconstructing a missing‐wedge X‐ray ptychographic tomography (PXCT) data set of a macroporous zeolite particle, for which only 51 projections over 70° could be collected. The GANrec recovered the 3D pore structure with reasonable quality for further analysis. This reconstruction concept can work universally for most of the ill‐posed inverse problems if the forward model is well defined, such as phase retrieval of in‐line phase‐contrast imaging.

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In this letter we report on the creation of hard X-ray beams carrying orbital angular momentum of topological charge −h and −3h at a photon energy of 8.2 keV via spiral phase plates made out of fused silica by ultrashort-pulsed laser ablation. The phase plates feature a smooth phase ramp with 0.5 µm nominal step height and a surface roughness of 0.5 µm. The measured vortex beams show sub-micrometer sized donut rings and agree well with numerical modeling. Fused silica phase plates are potentially suited to manipulate the electromagnetic field in highly intense X-ray beams at X-ray free-electron laser sources.

Three-dimensional (3D) x-ray microscopy by ptychographic tomography requires elaborate numerical reconstructions. We describe a coupled ptychography-tomography reconstruction algorithm and apply it to an experimental ptychographic x-ray computed tomography data set of a catalyst particle. Compared to the traditional sequential algorithm, in which ptychographic projections are reconstructed to serve as input for subsequent tomographic reconstruction, the coupled ptychography-tomography algorithm reconstructs the 3D volume with higher spatial resolution over a larger field of view. Coupling the data from different projections improves the overall reconstruction, and the ptychographic sampling in individual projections can be coarsened beyond the point of overlap between neighboring scan points, still leading to stable reconstructions.

Two in situ `nanoreactors' for high-resolution imaging of catalysts have been designed and applied at the hard X-ray nanoprobe endstation at beamline P06 of the PETRA III synchrotron radiation source. The reactors house samples supported on commercial MEMS chips, and were applied for complementary hard X-ray ptychography (23 nm spatial resolution) and transmission electron microscopy, with additional X-ray fluorescence measurements. The reactors allow pressures of 100 kPa and temperatures of up to 1573 K, offering a wide range of conditions relevant for catalysis. Ptychographic tomography was demonstrated at limited tilting angles of at least ±35° within the reactors and ±65° on the naked sample holders. Two case studies were selected to demonstrate the functionality of the reactors: (i) annealing of hierarchical nanoporous gold up to 923 K under inert He environment and (ii) acquisition of a ptychographic projection series at ±35° of a hierarchically structured macroporous zeolite sample under ambient conditions. The reactors are shown to be a flexible and modular platform for in situ studies in catalysis and materials science which may be adapted for a range of sample and experiment types, opening new characterization pathways in correlative multimodal in situ analysis of functional materials at work. The cells will presently be made available for all interested users of beamline P06 at PETRA III.