| Literature DB >> 35787558 |
A Descamps1, B K Ofori-Okai1, J K Baldwin2, Z Chen1, L B Fletcher1, S H Glenzer1, N J Hartley1, J B Hasting1, D Khaghani1, M Mo1, B Nagler1, V Recoules3, R Redmer4, M Schörner4, P Sun1, Y Q Wang2, T G White5, E E McBride1.
Abstract
High-resolution inelastic X-ray scattering is an established technique in the synchrotron community, used to investigate collective low-frequency responses of materials. When fielded at hard X-ray free-electron lasers (XFELs) and combined with high-intensity laser drivers, it becomes a promising technique for investigating matter at high temperatures and high pressures. This technique gives access to important thermodynamic properties of matter at extreme conditions, such as temperature, material sound speed, and viscosity. The successful realization of this method requires the acquisition of many identical laser-pump/X-ray-probe shots, allowing the collection of a sufficient number of photons necessary to perform quantitative analyses. Here, a 2.5-fold improvement in the energy resolution of the instrument relative to previous works at the Matter in Extreme Conditions (MEC) endstation, Linac Coherent Light Source (LCLS), and the High Energy Density (HED) instrument, European XFEL, is presented. Some aspects of the experimental design that are essential for improving the number of photons detected in each X-ray shot, making such measurements feasible, are discussed. A careful choice of the energy resolution, the X-ray beam mode provided by the XFEL, and the position of the analysers used in such experiments can provide a more than ten-fold improvement in the photometrics. The discussion is supported by experimental data on 10 µm-thick iron and 50 nm-thick gold samples collected at the MEC endstation at the LCLS, and by complementary ray-tracing simulations coupled with thermal diffuse scattering calculations. open access.Entities:
Keywords: XFEL; extreme conditions; high-resolution inelastic X-ray scattering; thermal diffuse scattering
Year: 2022 PMID: 35787558 PMCID: PMC9255572 DOI: 10.1107/S1600577522004453
Source DB: PubMed Journal: J Synchrotron Radiat ISSN: 0909-0495 Impact factor: 2.557
Figure 1Schematic of the experimental setup used to perform milli-electronvolt inelastic X-ray scattering at the MEC endstation at the LCLS. X-ray pulses at 10.896 keV are first monochromated using a four-bounce (931) silicon monochromator arranged in a non-dispersive configuration and positioned at a glancing angle of incidence of 87.9°. Monochromatic X-ray pulses are then incident on a 50 µm-thick PMMA sample. Scattered photons are finally collected by four diced (931) silicon analysers and focused on an ePix100 detector (Carini et al., 2016 ▸). The sample is oriented at a 22° angle such that the scattering vector Q is parallel to the [010] crystallographic direction at the 44° analyser location. The inset shows the raw data collected for each analyser. The curvature of the traces at Q = 4.1 Å−1 and Q = 4.8 Å−1 is postulated to arise from defocusing effects as these analysers could not be positioned at best focus.
Figure 2(a) Instrument functions measured on a 50 µm-thick PMMA sample at Q ≃ 2 Å−1 using the (533) reflection of silicon at 7.5 keV (orange diamonds) and the (931) reflection of silicon at 10.9 keV (black squares). The solid lines correspond to the best fit to the data assuming a pseudo-Voigt lineshape and the black dashed line shows the simulated instrument function. (b) Inelastic spectrum measured from a 10 µm-thick Fe sample at ambient conditions (dark squares) to highlight the effect of the improved energy resolution. The solid black line corresponds to the best fit to the data using the model described by Descamps et al. (2020 ▸). The orange line corresponds to the spectrum one would expect using the energy resolution demonstrated at 7.5 keV. In both figures, each symbol corresponds to one pixel on the X-ray detector.
Contributions to the energy resolution of the high-resolution spectrometer using a 50 µm-thick PMMA sample
The different contributions are defined by Huotari et al. (2005 ▸) and Moretti Sala et al. (2018 ▸).
| Contribution | Δ |
|---|---|
| Analyser Darwin width | 14 |
| Source size | 8 |
| Pixel size | 10 |
| Johann aberration | 5 |
| Spectrometer | 20 |
| Incident bandwidth | 11 |
| Total | 22 |
Figure 3(a) Example spectra of the SASE beam mode (orange) and the HXRSS beam mode (black). The faint lines correspond to single-shot spectra recorded using a bent silicon spectrometer upstream of the MEC endstation at the LCLS (Zhu et al., 2012 ▸). The thick lines correspond to the average spectra from 104 shots. For clarity, only 20 single-shot spectra are shown. (b) Number of photons scattered from a 50 µm-thick PMMA sample at Q = 3.5 Å−1 using the SASE beam mode (orange squares) and using the HXRSS beam mode (black squares). The solid line corresponds to a fit to the experimental data using a pseudo-Voigt lineshape.
Figure 4(a) Thermal diffuse scattering intensity calculated for gold, I TDS, as a function of the angular offset from the direct X-ray beam in the equatorial plane, 2θ. (b) Corresponding phonon dispersion relation. Blue corresponds to the longitudinal acoustic (LA) mode, orange and red correspond to the transverse acoustic (TA) modes. The solid black line in (a) corresponds to the summation over all the branches. The dashed vertical black lines in (a) and (b) represent the angular offset for the analysers used in the discussed experiment.
Figure 5(a) Inelastic X-ray scattering spectrum recorded on a 50 nm-thick textured Au sample at 2.1 Å−1 and at ambient conditions (black) along with ray-tracing simulations (orange). The measured instrument function is shown in gray for comparison. (b) Calculated thermal diffuse scattering intensity, I TDS, for equation (2) normalized by the value at 2.1 Å−1 (22°) (black) along with the experimentally recorded number of photons on the detector, N Det, normalized by the value at 2.1 Å−1 (orange squares).