Frederik Stöhr

Sacrificial structures for deep reactive ion etching of high-aspect ratio kinoform silicon x-ray lenses

This article describes the realization of complex high-aspect ratio silicon structures with feature dimensions from 100 μm to 100 nm by deep reactive ion etching using the Bosch process. As the exact shape of the sidewall profiles can be crucial for the proper functioning of a device, the authors investigated how sacrificial structures in the form of guarding walls and pillars may be utilized to facilitate accurate control of the etch profile. Unlike other sacrificial structuring approaches, no silicon-on-insulator substrates or multiple lithography steps are required. In addition, the safe removal of the sacrificial structures was accomplished by thermal oxidation and subsequent selective wet etching. The effects of the dimensions and relative placement of sacrificial walls and pillars on the etching result were determined through systematic experiments. The authors applied this process for exact sidewall control in the manufacture of x-ray lenses that are very sensitive to sidewall shape nonuniformities...

Optimizing shape uniformity and increasing structure heights of deep reactive ion etched silicon x-ray lenses

Line-focusing compound silicon x-ray lenses with structure heights exceeding 300 μm were fabricated using deep reactive ion etching. To ensure profile uniformity over the full height, a new strategy was developed in which the perimeter of the structures was defined by trenches of constant width. The remaining sacrificial material inside the lens cavities was removed by etching through the silicon wafer. Since the wafers become fragile after through-etching, they were then adhesively bonded to a carrier wafer. Individual chips were separated using laser micro machining and the 3D shape of fabricated lenses was thoroughly characterized by a variety of means. Optical testing using synchrotron radiation with a photon energy of 56 keV yielded a 300 μm wide beam with a waist of 980 nm (full width at half maximum) at a focal length of 1.3 m. Optical aberrations are discussed in the context of the shape analysis, where a slight bowing of the lens sidewalls and an insufficiently uniform apex region are identified as resolution-limiting factors. Despite these, the proposed fabrication route proved a viable approach for producing x-ray lenses with large structure heights and provides the means to improve the resolution and capabilities of modern x-ray techniques such as x-ray microscopy and 3D x-ray diffraction.

Dark field X-ray microscopy for studies of recrystallization

We present the recently developed technique of Dark Field X-Ray Microscopy that utilizes the diffraction of hard X-rays from individual grains or subgrains at the (sub)micrometre- scale embedded within mm-sized samples. By magnifying the diffracted signal, 3D mapping of orientations and strains inside the selected grain is performed with an angular resolution of 0.005o and a spatial resolution of 200 nm. Furthermore, the speed of the measurements at high- intensity synchrotron facilities allows for fast non-destructive in situ determination of structural changes induced by annealing or other external influences. The capabilities of Dark Field X- Ray Microscopy are illustrated by examples from an ongoing study of recrystallization of 50% cold-rolled Al1050 specimens.

Long-range symmetry breaking in embedded ferroelectrics

The characteristic functionality of ferroelectric materials is due to the symmetry of their crystalline structure. As such, ferroelectrics lend themselves to design approaches that manipulate this structural symmetry by introducing extrinsic strain. Using in situ dark-field X-ray microscopy to map lattice distortions around deeply embedded domain walls and grain boundaries in BaTiO3, we reveal that symmetry-breaking strain fields extend up to several micrometres from domain walls. As this exceeds the average domain width, no part of the material is elastically relaxed, and symmetry is universally broken. Such extrinsic strains are pivotal in defining the local properties and self-organization of embedded domain walls, and must be accounted for by emerging computational approaches to material design.Ferroelectricity can be modified by domain wall strain fields that extend over nanometres. Here, with X-ray microscopy, strain fields over several micrometres are observed in BaTiO3, suggesting ferroelectricity is globally altered throughout the material.

Injection molded polymeric hard X-ray lenses

A novel and economical approach for fabricating compound refractive lenses for the purpose of focusing hard X-rays is described. A silicon master was manufactured by UV-lithography and deep reactive ion etching (DRIE). Sacrificial structures were utilized, which enabled accurate control of the etching profile and were removed after DRIE. By electroplating, an inverse nickel sample was obtained, which was used as a mold insert in a commercial polymer injection molding machine. A prototype lens made of polyethylene with a focal length of 350 mm was tested using synchrotron radiation at photon energies of 17 keV. A 55 µm long line focus with a minimal waist of 770 nm (FWHM) and a total lens transmittance of 32% were measured. Due to its suitability for cheap mass production, this highly efficient optics may find widespread use in hard X-ray instruments.