Mapping the Pore Architecture of Structured Catalyst Monoliths from Nanometer to Centimeter Scale with Electron and X-ray Tomographies

The hierarchical pore systems of Pt/Al2O3 exhaust gas aftertreatment catalysts were analyzed with a collection of correlative imaging techniques to monitor changes induced by hydrothermal aging. Synergistic imaging with laboratory X-ray microtomography, synchrotron radiation ptychographic X-ray computed nanotomography, and electron tomography allowed quantitative observation of the catalyst pore architecture from centimeter to nanometer scale. Thermal aging at 750 °C in air and hydrothermal aging at 1050 °C in 10% H2O/air caused increasing structural degradation, which manifested as widespread sintering of Pt particles, increased volume and quantity of macropores (>20 nm), and reduction in effective surface area coupled with decreasing volume and frequency of mesopores (2-20 nm) and micropores (<2 nm). Electron tomography unraveled the three-dimensional (3D) structure with high resolution allowing visualization of meso- and macropores but with samples of maximum 300 nm thickness. To complement this, hard X-ray ptychographic tomography produced quantitative 3D electron density maps of 5 μm diameter samples with spatial resolution <50 nm, effectively filling the resolution gap between electron tomography and hard X-ray microtomography. The obtained 3D volumes are an essential input for future computational modeling of fluid dynamics, mass transport, or diffusion properties and may readily complement bulk one-dimensional porosimetry measurements or simulated porosity

Flexible plenoptic X-ray microscopy

X-ray computed tomography (CT) is an invaluable technique for generating three-dimensional (3D) images of inert or living specimens. X-ray CT is used in many scientific, industrial, and societal fields. Compared to conventional 2D X-ray imaging, CT requires longer acquisition times because up to several thousand projections are required for reconstructing a single high-resolution 3D volume. Plenoptic imaging—an emerging technology in visible light field photography—highlights the potential of capturing quasi-3D information with a single exposure. Here, we show the first demonstration of a flexible plenoptic microscope operating with hard X-rays; it is used to computationally reconstruct images at different depths along the optical axis. The experimental results are consistent with the expected axial refocusing, precision, and spatial resolution. Thus, this proof-of-concept experiment opens the horizons to quasi-3D X-ray imaging, without sample rotation, with spatial resolution of a few hundred nanometres

Refractive Lenses for Microscopy and Nanoanalysis

X-rays offer indispensable opportunities for science, medicine, and technology due to a large variety of exceptional properties. The large penetration depth of X-rays in matter allows one to investigate the inner structures of an object without destructive sample preparation, or inside special sample environments, such as chemical reactors or pressure cells. In this way, X-rays are ideally suited to study physical and chemical processes in situ and operando. In addition, X-ray analytical techniques, such as X-ray diffraction, fluorescence, and absorption, provide atomic-scale structure information, elemental concentrations, and the chemical state of a given elemental species inside the sample. With the advent of highly brilliant synchrotron radiation sources of the third generation, it became possible to combine X-ray analytics with microscopy, triggering the rapid development of new types of optics for X-rays, amongst which refractive X-ray lenses have progressed at a spectacular pace

Refractive hard x-ray vortex phase plates

In this Letter, we report on the creation of hard x-ray beams carrying orbital angular momentum of topological charge −ℏ and −3ℏ 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 a 0.5 μm nominal step height and a surface roughness of 0.5 μm. The measured vortex beams show submicrometer-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

Diamond nanofocusing refractive X-ray lenses made by planar etching technology

The manufacturing steps and first tests of a refractive lens made of polycrystalline diamond are described. A fabrication process based on electron-beam lithography and deep reactive ion etching is introduced. Experimental tests on beamline ID13 at the ESRF have been performed. A spot size of 360 nm (FWHM) at an energy E = 24.3 keV is observed

Ptychographic characterization of polymer compound refractive lenses manufactured by additive technology

The recent success in the development of high-precision printing techniques allows one to manufacture free-standing polymer structures of high quality. Two-photon polymerization lithography is a mask-less technique with down to 100 nm resolution that provides full geometric freedom. It has recently been applied to the nanofabrication of X-ray compound refractive lenses (CRLs). In this article we report on the characterization of two sets of CRLs of different design produced by two-photon polymerization-induced lithography