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.

Point focusing with flat and wedged crossed multilayer Laue lenses.

Point focusing measurements using pairs of directly bonded crossed multilayer Laue lenses (MLLs) are reported. Several flat and wedged MLLs have been fabricated out of a single deposition and assembled to realise point focusing devices. The wedged lenses have been manufactured by adding a stress layer onto flat lenses. Subsequent bending of the structure changes the relative orientation of the layer interfaces towards the stress-wedged geometry. The characterization at ESRF beamline ID13 at a photon energy of 10.5 keV demonstrated a nearly diffraction-limited focusing to a clean spot of 43 nm × 44 nm without significant side lobes with two wedged crossed MLLs using an illuminated aperture of approximately 17 µm × 17 µm to eliminate aberrations originating from layer placement errors in the full 52.7 µm × 52.7 µm aperture. These MLLs have an average individual diffraction efficiency of 44.5%. Scanning transmission X-ray microscopy measurements with convenient working distances were performed to demonstrate that the lenses are suitable for user experiments. Also discussed are the diffraction and focusing properties of crossed flat lenses made from the same deposition, which have been used as a reference. Here a focal spot size of 28 nm × 33 nm was achieved and significant side lobes were noticed at an illuminated aperture of approximately 23 µm × 23 µm.

Ptychography with multilayer Laue lenses.

Two different multilayer Laue lens designs were made with total deposition thicknesses of 48 µm and 53 µm, and focal lengths of 20.0 mm and 12.5 mm at 20.0 keV, respectively. From these two multilayer systems, several lenses were manufactured for one- and two-dimensional focusing. The latter is realised with a directly bonded assembly of two crossed lenses, that reduces the distance between the lenses in the beam direction to 30 µm and eliminates the necessity of producing different multilayer systems. Characterization of lens fabrication was performed using a laboratory X-ray microscope. Focusing properties have been investigated using ptychography.

Full-field X-ray microscopy with crossed partial multilayer Laue lenses.

We demonstrate full-field X-ray microscopy using crossed multilayer Laue lenses (MLL). Two partial MLLs are prepared out of a 48 µm high multilayer stack consisting of 2451 alternating zones of WSi2 and Si. They are assembled perpendicularly in series to obtain two-dimensional imaging. Experiments are done in a laboratory X-ray microscope using Cu-Kα radiation (E = 8.05 keV, focal length f = 8.0 mm). Sub-100 nm resolution is demonstrated without mixed-order imaging at an appropriate position of the image plane. Although existing deviations from design parameters still cause aberrations, MLLs are a promising approach to realize hard X-ray microscopy at high efficiencies with resolutions down to the sub-10 nm range in future.

Kinoform diffractive lenses for efficient nano-focusing of hard X-rays.

A nano-focusing module based on two linear Fresnel zone plates is presented. The zone plates are designed to generate a kinoform phase profile in tilted geometry, thus overcoming the efficiency limitations of binary diffractive structures. Adjustment of the tilt angle enables tuning of the setup for optimal efficiency over a wide range of photon energies, ranging from 5 to 20 keV. Diffraction efficiency of more than 50% was measured for the full module at 8 keV photon energy. A diffraction limited spot size of 100 nm was verified by ptychographic reconstruction for a lens module with a large entrance aperture of 440 µm × 400 µm.

Damage investigation on tungsten and diamond diffractive optics at a hard x-ray free-electron laser.

Focusing hard x-ray free-electron laser radiation with extremely high fluence sets stringent demands on the x-ray optics. Any material placed in an intense x-ray beam is at risk of being damaged. Therefore, it is crucial to find the damage thresholds for focusing optics. In this paper we report experimental results of exposing tungsten and diamond diffractive optics to a prefocused 8.2 keV free-electron laser beam in order to find damage threshold fluence levels. Tungsten nanostructures were damaged at fluence levels above 500 mJ/cm(2). The damage was of mechanical character, caused by thermal stress variations. Diamond nanostructures were affected at a fluence of 59 000 mJ/cm(2). For fluence levels above this, a significant graphitization process was initiated. Scanning Electron Microscopy (SEM) and µ-Raman analysis were used to analyze exposed nanostructures.

Ronchi test for characterization of nanofocusing optics at a hard x-ray free-electron laser.

We demonstrate the use of the classical Ronchi test to characterize aberrations in focusing optics at a hard x-ray free-electron laser. A grating is placed close to the focus and the interference between the different orders after the grating is observed in the far field. Any aberrations in the beam or the optics will distort the interference fringes. The method is simple to implement and can provide single-shot information about the focusing quality. We used the Ronchi test to measure the aberrations in a nanofocusing Fresnel zone plate at the Linac Coherent Light Source at 8.194 keV.

Full optical characterization of coherent x-ray nanobeams by ptychographic imaging.

Scanning coherent diffraction microscopy (ptychography) is an emerging hard x-ray microscopy technique that yields spatial resolutions well below the lateral size of the probing nanobeam. Besides a high resolution image of the object, the complex wave field of the probe can be reconstructed at the position of the object. By verifying the consistency of several independent wave field measurements along the optical axis, we address the question of how well the reconstruction represents the nanobeam. With a single ptychogram the wave field can be properly determined over a large range along the optical axis, also at positions inaccessible otherwise.

Beamstop-based low-background ptychography to image weakly scattering objects.

In recent years, X-ray ptychography has been established as a valuable tool for high-resolution imaging. Nevertheless, the spatial resolution and sensitivity in coherent diffraction imaging are limited by the signal that is detected over noise and over background scattering. Especially, coherent imaging of weakly scattering specimens suffers from incoherent background that is generated by the interaction of the central beam with matter along its propagation path in particular close to and inside of the detector. Common countermeasures entail evacuated flight tubes or detector-side beamstops, which improve the experimental setup in terms of background reduction or better coverage of high dynamic range in the diffraction patterns. Here, we discuss an alternative approach: we combine two ptychographic scans with and without beamstop and reconstruct them simultaneously taking advantage of the complementary information contained in the two scans. We experimentally demonstrate the potential of this scheme for hard X-ray ptychography by imaging a weakly scattering object composed of catalytic nanoparticles and provide the analysis of the signal-to-background ratio in the diffraction patterns.

X-rays Reveal the Internal Structure of Keratin Bundles in Whole Cells.

In recent years, X-ray imaging of biological cells has emerged as a complementary alternative to fluorescence and electron microscopy. Different techniques were established and successfully applied to macromolecular assemblies and structures in cells. However, while the resolution is reaching the nanometer scale, the dose is increasing. It is essential to develop strategies to overcome or reduce radiation damage. Here we approach this intrinsic problem by combing two different X-ray techniques, namely ptychography and nanodiffraction, in one experiment and on the same sample. We acquire low dose ptychography overview images of whole cells at a resolution of 65 nm. We subsequently record high-resolution nanodiffraction data from regions of interest. By comparing images from the two modalities, we can exclude strong effects of radiation damage on the specimen. From the diffraction data we retrieve quantitative structural information from intracellular bundles of keratin intermediate filaments such as a filament radius of 5 nm, hexagonal geometric arrangement with an interfilament distance of 14 nm and bundle diameters on the order of 70 nm. Thus, we present an appealing combined approach to answer a broad range of questions in soft-matter physics, biophysics and biology.

Imaging Shock Waves in Diamond with Both High Temporal and Spatial Resolution at an XFEL.

The advent of hard x-ray free-electron lasers (XFELs) has opened up a variety of scientific opportunities in areas as diverse as atomic physics, plasma physics, nonlinear optics in the x-ray range, and protein crystallography. In this article, we access a new field of science by measuring quantitatively the local bulk properties and dynamics of matter under extreme conditions, in this case by using the short XFEL pulse to image an elastic compression wave in diamond. The elastic wave was initiated by an intense optical laser pulse and was imaged at different delay times after the optical pump pulse using magnified x-ray phase-contrast imaging. The temporal evolution of the shock wave can be monitored, yielding detailed information on shock dynamics, such as the shock velocity, the shock front width, and the local compression of the material. The method provides a quantitative perspective on the state of matter in extreme conditions.

Full spatial characterization of a nanofocused x-ray free-electron laser beam by ptychographic imaging.

The emergence of hard X-ray free electron lasers (XFELs) enables new insights into many fields of science. These new sources provide short, highly intense, and coherent X-ray pulses. In a variety of scientific applications these pulses need to be strongly focused. In this article, we demonstrate focusing of hard X-ray FEL pulses to 125 nm using refractive x-ray optics. For a quantitative analysis of most experiments, the wave field or at least the intensity distribution illuminating the sample is needed. We report on the full characterization of a nanofocused XFEL beam by ptychographic imaging, giving access to the complex wave field in the nanofocus. From these data, we obtain the full caustic of the beam, identify the aberrations of the optic, and determine the wave field for individual pulses. This information is for example crucial for high-resolution imaging, creating matter in extreme conditions, and nonlinear x-ray optics.

Scanning X-ray nanodiffraction: from the experimental approach towards spatially resolved scattering simulations.

: An enhancement on the method of X-ray diffraction simulations for applications using nanofocused hard X-ray beams is presented. We combine finite element method, kinematical scattering calculations, and a spot profile of the X-ray beam to simulate the diffraction of definite parts of semiconductor nanostructures. The spot profile could be acquired experimentally by X-ray ptychography. Simulation results are discussed and compared with corresponding X-ray nanodiffraction experiments on single SiGe dots and dot molecules.

Grazing incidence small-angle X-ray scattering microtomography demonstrated on a self-ordered dried drop of nanoparticles.

We combine grazing-incidence small-angle X-ray scattering (GISAXS) with scanning X-ray microtomography to investigate the nanostructure in a dried gold/polystyrene nanocomposite drop. Local GISAXS structure factors are reconstructed at each position on the surface of this two-dimensionally heterogeneous sample with 30 microm pixel size. Evidence for four types of self-assembled colloidal crystalline structures is provided by the reconstructed data of the drop demonstrating the feasibility of the method.