We present an improved nanofabrication method of high aspect ratio tungsten structures for use in high efficiency nanofocusing hard X-ray zone plates. A ZEP 7000 electron beam resist layer used for patterning is cured by a second, much larger electron dose after development. The curing step improves pattern transfer fidelity into a chromium hard mask by reactive ion etching using Cl2/O2 chemistry. The pattern can then be transferred into an underlying tungsten layer by another reactive ion etching step using SF6/O2. A 630 nm-thick tungsten zone plate with smallest line width of 30 nm was fabricated using this method and characterized. At 8.2 keV photon energy the device showed an efficiency of 2.2% with a focal spot size at the diffraction limit, measured at Diamond Light Source I-13-1 beamline.

Metal-assisted chemical etching (MACE) reaction parameters were investigated for the fabrication of specially designed silicon-based x-ray zone plate nanostructures using a gold catalyst pattern and etching solutions composed of HF and H2O2. Etching depth, zone verticality and zone roughness were studied as a function of etching solution composition, temperature and processing time. Homogeneous, vertical etching with increasing depth is observed at increasing H2O2 concentrations and elevated processing temperatures, implying a balance in the hole injection and silica dissolution kinetics at the gold-silicon interface. The etching depth decreases and zone roughness increases at the highest investigated H2O2 concentration and temperature. Possible reasons for these observations are discussed based on reaction chemistry and zone plate design. Optimum MACE conditions are found at HF:H2O2 concentrations of 4.7 M:0.68 M and room temperature with an etching rate of 0.7 micrometers per minute, which is about an order of magnitude higher than previous reports. Moreover, our results show that a grid catalyst design is important for successful fabrication of vertical high aspect ratio silicon nanostructures.

We present our results in fabricating Fresnel zone plate optics for the NanoMAX beamline at the fourth-generation synchrotron radiation facility MAX IV, to be used in the energy range of 6-10 keV. The results and challenges of tungsten nanofabrication are discussed, and an alternative approach using metal-assisted chemical etching (MACE) of silicon is showcased. We successfully manufactured diffraction-limited zone plates in tungsten with 30 nm outermost zone width and an aspect ratio of 21:1. These optics were used for nanoimaging experiments at NanoMAX. However, we found it challenging to further improve resolution and diffraction efficiency using tungsten. High efficiency is desirable to fully utilize the advantage of increased coherence on the optics at MAX IV. Therefore, we started to investigate MACE of silicon for the nanofabrication of high-resolution and high-efficiency zone plates. The first type of structures we propose use the silicon directly as the phase-shifting material. We have achieved 6 mu m deep dense vertical structures with 100 nm linewidth. The second type of optics use iridium as the phase material. The structures in the silicon substrate act as a mold for iridium coating via atomic layer deposition (ALD). A semi-dense pattern is used with line-to-space ratio of 1:3 for a so-called frequency-doubled zone plate. This way, it is possible to produce smaller structures with the tradeoff of the additional ALD step. We have fabricated 45 nm-wide and 3.6 mu m-tall silicon/iridium structures.

Due to their short wavelength, X-rays can in principle be focused down to a few nanometres and below. At the same time, it is this short wavelength that puts stringent requirements on X-ray optics and their metrology. Both are limited by today’s technology. In this work, we present accurate at wavelength measurements of residual aberrations of a refractive X-ray lens using ptychography to manufacture a corrective phase plate. Together with the fitted phase plate the optics shows diffraction-limited performance, generating a nearly Gaussian beam profile with a Strehl ratio above 0.8. This scheme can be applied to any other focusing optics, thus solving the X-ray optical problem at synchrotron radiation sources and X-ray free-electron lasers.

NanoMAX is a hard x-ray nanoimaging beamline at the new Swedish synchrotron radiation source MAX IV that became operational in 2016. Being a beamline dedicated to x-ray nanoimaging in both 2D and 3D, NanoMAX is the first to take full advantage of MAX IVs exceptional low emittance and resulting coherent properties. We present results from the first experiments at NanoMAX that took place in December 2016. These did not use the final experimental stations that will become available to users, but a temporary arrangement including zone plate and order-sorting aperture stages and a piezo-driven sample scanner. We used zone plates with outermost zone widths of 100 nm and 30 nm and performed experiments at 8 keV photon energy for x-ray absorption and fluorescence imaging and ptychography. Moreover, we investigated stability and coherence with a Ronchi test method. Despite the rather simple setup, we could demonstrate spatial resolution below 50 nm after only a few hours of beamtime. The results showed that the beamline is working as expected and experiments approaching the 10 nm resolution level or below should be possible in the future.