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A parallel paper [Berujon, Cojocaru, Piault, Celestre, Roth, Barrett & Ziegler (2020), J. Synchrotron Rad. 27, 284-292] reviewed theoretically some of the available processing schemes for X-ray wavefront sensing based on random modulation. Shown here are experimental applications of the technique for characterizing both refractive and reflective optical components. These fast and accurate X-ray at-wavelength metrology methods can assist the manufacture of X-ray optics that transport X-ray beams with a minimum amount of wavefront distortion. It is also recalled how such methods can facilitate online optimization of active optics.

X-ray near-field speckle-based phase-sensing approaches provide efficient means of characterizing optical elements. Presented here is a theoretical review of several of these speckle methods within the framework of optical characterization, and a generalization of the concept is provided. As is also demonstrated experimentally in a parallel paper [Berujon, Cojocaru, Piault, Celestre, Roth, Barrett & Ziegler (2020), J. Synchrotron Rad. 27, (this issue)], the methods theoretically developed here can be applied to different beams and optics and within a variety of situations where at-wavelength metrology is desired. By understanding the differences between the various processing methods, it is possible to find and implement the most suitable approach for each metrology scenario.

Here a direct comparison is made between various X-ray wavefront sensing methods with application to optics alignment and focus characterization at X-ray free-electron lasers (XFELs). Focus optimization at XFEL beamlines presents unique challenges due to high peak powers as well as beam pointing instability, meaning that techniques capable of single-shot measurement and that probe the wavefront at an out-of-focus location are desirable. The techniques chosen for the comparison include single-phase-grating Talbot interferometry (shearing interferometry), dual-grating Talbot interferometry (moiré deflectometry) and speckle tracking. All three methods were implemented during a single beam time at the Linac Coherent Light Source, at the X-ray Pump Probe beamline, in order to make a direct comparison. Each method was used to characterize the wavefront resulting from a stack of beryllium compound refractive lenses followed by a corrective phase plate. In addition, difference wavefront measurements with and without the phase plate agreed with its design to within λ/20, which enabled a direct quantitative comparison between methods. Finally, a path toward automated alignment at XFEL beamlines using a wavefront sensor to close the loop is presented., (open access.)

An instrument allowing the quantitative analysis of X-ray pulsed wavefronts is presented and its processing method explained. The system relies on the X-ray speckle tracking principle to accurately measure the phase gradient of the X-ray beam from which beam optical aberrations can be deduced. The key component of this instrument, a semi-transparent scintillator emitting visible light while transmitting X-rays, allows simultaneous recording of two speckle images at two different propagation distances from the X-ray source. The speckle tracking procedure for a reference-less metrology mode is described with a detailed account on the advanced processing schemes used. A method to characterize and compensate for the imaging detector distortion, whose principle is also based on speckle, is included. The presented instrument is expected to find interest at synchrotrons and at the new X-ray free-electron laser sources under development worldwide where successful exploitation of beams relies on the availability of an accurate wavefront metrology.

X-ray diffraction techniques are used in imaging mode in order to characterize micrometre-sized objects. The samples used as models are metal-oxide tunnel junctions made by optical lithography, with lateral sizes ranging from 150 µm down to 10 µm and various shapes: discs, squares and rectangles. Two approaches are described and compared, both using diffraction contrast: full-field imaging (topography) and raster imaging (scanning probe) using a micrometre-sized focused X-ray beam. It is shown that the full-field image gives access to macroscopic distortions (e.g. sample bending), while the local distortions, at the micrometre scale (e.g. tilts of the crystalline planes in the vicinity of the junction edges), can be accurately characterized only using focused X-ray beams. These local defects are dependent on the junction shape and larger by one order of magnitude than the macroscopic curvature of the sample.

A method for the fabrication of linear transmission Fresnel zone plates for X-rays in the 8-15 keV photon energy range is presented. The diffractive elements are generated by electron-beam lithography and chemical wet etching of (110)-oriented silicon membrane substrates. Diffractive structures with aspect ratios of more than 30 for 300 nm-wide structures were obtained. The diffraction efficiency of such a lens was measured for 13.3 keV radiation to be 20%.

Magnetic reflectometry experiments have been performed in the X-ray range at the L(2,3) edges of rhodium. What makes these experiments original is the insertion of a very compact double-bounce reflectometer upstream of the monochromator. This configuration makes full use of the high polarization rate of the helical undulator source. This advantage is reflected in the high quality of the data obtained after only a few accumulations. It is also shown that, by properly selecting the angle of incidence, one may obtain experimental differential X-ray reflectivity spectra dominated either by the dispersion or the absorption terms.