Hybrid diamond-silicon angular-dispersive x-ray monochromator with 0.25-meV energy bandwidth and high spectral efficiency.

We report on the design, implementation, and performance of an x-ray monochromator with ultra-high energy resolution (ΔE/E ≃ 2.7 × 10(-8)) and high spectral efficiency using x rays with photon energies E ≃ 9.13 keV. The operating principle of the monochromator is based on the phenomenon of angular dispersion in Bragg back-diffraction. The optical scheme of the monochromator is a modification of a scheme reported earlier [Shvyd'ko et al., Phys. Rev. A 84, 053823 (2011)], where a collimator/wavelength selector Si crystal was replaced with a 100-µm-thick type IIa diamond crystal. This modification provides a very-small-energy bandwidth ΔE ≃ 0.25 meV, a 3-fold increase in the aperture of the accepted beam, a reduction in the cumulative angular dispersion rate of x rays emanating from the monochromator for better focusing on a sample, a sufficient angular acceptance matching the angular divergence of an undulator source (≈ 10 µrad), and an improved throughput due to low x-ray absorption in the thin diamond crystal. The measured spectral efficiency of the monochromator was ≈ 65% with an aperture of 0.3 × 1 mm(2). The performance parameters of the monochromator are suitable for inelastic x-ray spectroscopy with an absolute energy resolution ΔE < 1 meV.

Fluorescence detection of white-beam X-ray absorption anisotropy: towards element-sensitive projections of local atomic structure.

Projections of the atomic structure around Nb atoms in a LiNbO(3) single crystal were obtained from a white-beam X-ray absorption anisotropy (XAA) pattern detected using Nb K fluorescence. This kind of anisotropy results from the interference of X-rays inside a sample and, owing to the short coherence length of a white beam, is visible only at small angles around interatomic directions. Consequently, the main features of the recorded XAA corresponded to distorted real-space projections of dense-packed atomic planes and atomic rows. A quantitative analysis of XAA was carried out using a wavelet transform and allowed well resolved projections of Nb atoms to be obtained up to distances of 10 Å. The signal of nearest O atoms was detected indirectly by a comparison with model calculations. The measurement of white-beam XAA using characteristic radiation indicates the possibility of obtaining element-sensitive projections of the local atomic structure in more complex samples.

A high-pressure single-crystal synchrotron diffraction study of NH4RbTe4O9·2H2O: stability of three different TeO(x) coordination polyhedra.

The crystal structure of ammonium rubidium nonaoxotetratellurate(IV) dihydrate has been studied as a function of pressure up to 7.40 GPa. The ambient-pressure structure is characterized by the co-existence of three different Te-O polyhedra (TeO(3), TeO(4) and TeO(5)), which are connected to form layers. NH(4)(+), H(2)O and Rb(+) are incorporated between the layers. Both the Rb1 position, which is located on a twofold axis, and the Rb2 position are partially occupied. The three different types of coordination polyhedra around Te(4+) are stable up to at least 5.05 GPa. No phase transition is observed. The fit of the unit-cell volume as a function of pressure gives a zero-pressure bulk modulus of 34 (1) GPa with a zero-pressure volume of V(0) = 2620 (4) Å(3) [B' = 1.4 (2)].

Diffraction properties of periodic lattices under free electron laser radiation.

In this Letter, we report the pioneering use of free electron laser radiation for the investigation of periodic crystalline structures. The diffraction properties of silver behenate single nanocrystals (5.8 nm periodicity) with the dimensions of 20 nm x 20 nm x 20 microm and as powder with grain sizes smaller than 200 nm were investigated with 8 nm free electron laser radiation in single-shot modus with 30 fs long free electron laser pulses. This work emphasizes the possibility of using soft x-ray free electron laser radiation for these crystallographic studies on a nanometer scale.

X-ray tomographic imaging of crystal structure at the atomic level.

A direct nondiffractive tomographic algorithm is proposed for the determination of the crystal structure from real-space projections obtained by illuminating the sample with white x rays. This approach was applied to the pattern of the directional fine structure in absorption of white x rays recorded for a GaP crystal and allowed for a determination of the electron density distribution within the unit cell.