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Static phase shifters have been intensely studied for generating two- and three-dimensional electron beam patterns. However, those are restricted to specific electron beam energies and microscope settings. Aiming at overcoming such limitations, the development of programmable phase shifters based on e.g. a Boersch phase is an active field of research. We recently demonstrated a three-element Boersch phase shifter device [Thakkar et al., J. Appl. Phys.128, 134502 (2020)], which was fabricated by electron beam lithography and is compatible with up-scaling. However, it suffers from parasitic beam deflection and cross-talk. Here, we report a five-layer phase shifter device, which is based on a metal–insulator–metal–insulator–metal structure as originally envisioned by Boersch that reduces cross-talk. We demonstrate a three-element Boersch phase shifter that shows minimal beam deflection of voltage-controlled three-electron-beam interference patterns in a transmission electron microscope operated at 200 keV. The feasibility of using such multi-element phase shifter arrays is discussed in this article.

The availability of intense soft x-ray beams with tunable energy and polarization has pushed the development of highly sensitive, element-specific, and noninvasive microscopy techniques to investigate condensed matter with high spatial and temporal resolution. The short wavelengths of soft x-rays promise to reach spatial resolutions in the deep single-digit nanometer regime, providing unprecedented access to magnetic phenomena at fundamental length scales. Despite considerable efforts in soft x-ray microscopy techniques, a two-dimensional resolution of 10 nm has not yet been surpassed in direct imaging. Here, we report on a significant step beyond this long-standing limit by combining newly developed soft x-ray Fresnel zone plate lenses with advanced precision in scanning control and careful optical design. With this approach, we achieve an image resolution of 7 nm. By combining this highly precise microscopy technique with the x-ray magnetic circular dichroism effect, we reveal dimensionality effects in an ensemble of interacting magnetic nanoparticles. Such effects are topical in current nanomagnetism research and highlight the opportunities of high-resolution soft x-ray microscopy in magnetism research and beyond.

High aspect ratio nanostructuring requires high precision pattern transfer with highly directional etching. In this work, we demonstrate the fabrication of structures with ultra-high aspect ratios (up to 10 000 : 1) in the nanoscale regime (down to 10 nm) by platinum assisted chemical etching of silicon in the gas phase. The etching gas is created by a vapour of water diluted hydrofluoric acid and a continuous air flow, which works both as an oxidizer and as a gas carrier for reactive species. The high reactivity of platinum as a catalyst and the formation of platinum silicide to improve the stability of the catalyst pattern allow a controlled etching. The method has been successfully applied to produce straight nanowires with section size in the range of 10–100 nm and length of hundreds of micrometres, and X-ray optical elements with feature sizes down to 10 nm and etching depth in the range of tens of micrometres. This work opens the possibility of a low cost etching method for stiction-sensitive nanostructures and a large range of applications where silicon high aspect ratio nanostructures and high precision of pattern transfer are required.

We report on the fabrication of very high-resolution discrete four-resist-level grayscale patterns in poly(methyl methacrylate) with just 6-nm step height and down to 32-nm step width using dose-modulated, grayscale electron beam lithography and a low-contrast resist-developer system. This direct pattern writing is important for replication in high-volume manufacturing of diffractive optics. An innovative concept of unexposed auxiliary spacers helped to enhance the discrete character of the multi-level patterns. For pattern step widths between 100 and 32 nm, a transformation toward blazed gratings with increasingly continuous-slope character was obtained. All high-resolution patterns were prepared in a single exposure and development process from an initially about 30-nm thin film. The pattern roughness due to a relatively large polymer molecular weight was reduced using selective thermal annealing with only minimally affecting the global pattern shape by reflow. The results will enable further approaches toward single-digit vertical and prospectively single-digit lateral resolution grayscale patterns.

Photoelectrochemical (PEC) solar water splitting is a promising approach to convert solar energy into sustainable hydrogen fuel using semiconductor electrodes. Owing to their visible light absorption properties, oxynitrides have shown to be attractive photocatalysts for this application. In this study, the influence of the preparation method of CaNbO2N particles on their morphological and optical properties, and thereby their PEC performance, is investigated. The best performing CaNbO2N photoanode is produced by ammonolysis of Nb-enriched calcium niobium oxide. The enhanced photoactivity arises from an enlarged surface area and superior visible light absorption properties. The photoactivity of this photoanode was further enhanced by photodeposition of CoPi cocatalyst and by the atomic layer deposition of an Al2O3overlayer. A photocurrent density of 70 μA cm–2at 1.23 V versus reversible hydrogen electrode was achieved. The observed enhancement of the PEC performance after CoPi/Al2O3deposition is the combined effect of the improved kinetics of oxygen evolution because of the CoPi cocatalyst and the reduced surface recombination of the photogenerated carriers at the Al2O3surface layer.

Macromolecular crystallography often requires focused high-intensity x-ray beams for solving challenging protein structures from micrometer-sized crystals using current synchrotron radiation sources. The design of optical focusing schemes for hard x-rays showing high efficiency and flexibility in beam size is therefore continuously pursued. Here, we present an innovative solution based on a two-stage demagnification of the undulator source for photon energies from 6 keV to 19 keV, commissioned at the X10SA beamline of the Swiss Light Source, where a secondary source is imaged by two crossed silicon kinoform x-ray diffractive lenses with 75 nm outermost zone width. A source-size limited spot with a size of 4.8  μm×1.7  μm(h×v,FWHM) and flux of 7.5×10^10  photons/s at 12.4 keV is demonstrated at the sample position.

The focusing efficiency of conventional diffractive x-ray lenses is fundamentally limited due to their symmetric binary structures and the corresponding symmetry of their focusing and defocusing diffraction orders. Fresnel zone plates with asymmetric structure profiles can break this limitation; yet existing implementations compromise either on resolution, ease of use, or stability. We present a new way for the fabrication of such blazed lenses by patterning two complementary binary Fresnel zone plates on the front and back sides of the same membrane chip to provide a compact, inherently stable, single-chip device. The presented blazed double-sided zone plates with 200 nm smallest half-pitch provide up to 54.7% focusing efficiency at 6.2 keV, which is clearly beyond the value obtainable by their binary counterparts.

Phase contrast x-ray imaging (PCXI) is a promising imaging modality, capable of sensitively differentiating soft tissue structures at high spatial resolution. However, high sensitivity often comes at the cost of a long exposure time or multiple exposures per image, limiting the imaging speed and possibly increasing the radiation dose. Here, we demonstrate a PCXI method that uses a single short exposure to sensitively capture sample phase information, permitting high speed x-ray movies and live animal imaging. The method illuminates a checkerboard phase grid to produce a fine grid-like intensity reference pattern at the detector, then spatially maps sample-induced distortions of this pattern to recover differential phase images of the sample. The use of a phase grid is an improvement on our previous absorption grid work in two ways. There is minimal loss in x-ray flux, permitting faster imaging, and, a very fine pattern is produced for homogenous high spatial resolution. We describe how this pattern permits retrieval of five images from a single exposure; the sample phase gradient images in the horizontal and vertical directions, a projected phase depth image, an edge-enhanced image, and a type of scattering image. Finally, we describe how the reconstruction technique can achieve subpixel distortion retrieval and study the behavior of the technique in regard to analysis technique, Talbot distance, and exposure time.

Silicon nanowire field-effect transistors have attracted substantial interest for various biochemical sensing applications, yet there remains uncertainty concerning their response to changes in the supporting electrolyte concentration. In this study, we use silicon nanowires coated with highly pH-sensitive hafnium oxide (HfO2) and aluminum oxide (Al2O3) to determine their response to variations in KCl concentration at several constant pH values. We observe a nonlinear sensor response as a function of ionic strength, which is independent of the pH value. Our results suggest that the signal is caused by the adsorption of anions (Cl–) rather than cations (K+) on both oxide surfaces. By comparing the data to three well-established models, we have found that none of those can explain the present data set. Finally, we propose a new model which gives excellent quantitative agreement with the data.

Recent advances in the fabrication of diffractive X-ray optics have boosted hard X-ray microscopy into spatial resolutions of 30 nm and below. Here, we demonstrate the fabrication of zone-doubled Fresnel zone plates for multi-keV photon energies (4-12 keV) with outermost zone widths down to 20 nm. However, the characterization of such elements is not straightforward using conventional methods such as knife edge scans on well-characterized test objects. To overcome this limitation, we have used ptychographic coherent diffractive imaging to characterize a 20 nm-wide X-ray focus produced by a zone-doubled Fresnel zone plate at a photon energy of 6.2 keV. An ordinary scanning transmission X-ray microscope was modified to acquire the ptychographic data from a strongly scattering test object. The ptychographic algorithms allowed for the reconstruction of the image of the test object as well as for the reconstruction of the focused hard X-ray beam waist, with high spatial resolution and dynamic range. This method yields a full description of the focusing performance of the Fresnel zone plate and we demonstrate the usefulness ptychographic coherent diffractive imaging for metrology and alignment of nanofocusing diffractive X-ray lenses.

We fabricate computer generated holograms for the generation of phase singularities at extreme ultraviolet (EUV) wavelengths using electron beam lithography and demonstrate their ability to generate optical vortices in the nonzero diffraction orders. To this end, we observe the characteristic intensity distribution of the vortex beam and verify the helical phase structure interferometrically. The presented method forms the basis for further studies on singular light fields in the EUV frequency range, i.e., in EUV interference lithography. Since the method is purely achromatic, it may also find applications in various fields of x ray optics.