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Condens. Matter 2021, 6, 27 8 of 11 might lie in the long-range order. Moreover, the interstitial water in CuNP·2H2O may compete with Na-ions and hinder the ion intercalation process, while the Li-ion shuttling might not be affected due to its much lower ionic radius and the possibility to be inserted insmallercavities(rLi+ =0.77·rNa+).AlthoughtheelectrochemicalperformanceofCuNP does not compete with other candidates for Li-ion or Na-ion batteries, this work contributes to the overall scientific knowledge on the PBA materials and their possible use as host materials in energy storage applications. 4. Materials and Methods The synthesis of copper nitroprusside was partially based on a co-precipitation method reported in the literature [12,13]. Briefly, the co-precipitation occurred from 20 mM solutions of CuSO4·5H2O and Na2[Fe(CN)5(NO)]·2H2O, used as purchased by Sigma Aldrich. The simultaneous addition took place either at 40 ◦C (anhydrous sample) or 0 ◦C (hydrated sample) under constant stirring. The suspension was aged for two days, and the precipitate was collected by centrifugation. After that, the product was placed either directly in a desiccator (hydrated sample) or vacuum-dried at 60 ◦C overnight (anhydrous sample). X-ray diffraction (XRD) patterns were recorded at Elettra–Sincrotrone Trieste (Italy) at the MCX beamline [19] using a monochromatic beam of 1.033 Å. The storage ring operated at 2.0 GeV in top-up mode with a typical current of 310 mA. Data were collected in capillary mode consecutively from 10◦ to 70◦ 2θ-range with a 0.01◦ step and 0.5 s/point acquisition time. The XRD data analysis was performed using GSAS-II software [20], assuming as structural models the ones reported by Gómez et al. [15]. Instrumental parameters were retrieved from the XRD pattern of a silicon standard powder. Hence, instrumental broadening parameters, i.e., U, V, W, X and Y, were kept fixed during the successive XRD sample refinement. Peak shape was refined by optimizing the microstrain broadening parameter due to the sample only. Cell indexing was first conducted on the XRD patterns to determine the most appropriate space group. The refinement for the hydrated structure was performed in the 5–62.1938◦ 2θ-range, while the 5–62.2076◦ range was used for the anhydrous compound (dmin ~ 1.01 Å). Pawley refinement was achieved by considering the previously indexed cell and by refining a chebyschev background function, the unit cell parameters, and the microstrain (μstrain) in this order. Either an isotropic or a generalized μstrain model was used to model the peak shape and the results deriving from both models are reported in the Supplementary Information. After the Pawley refinement, charge flipping was carried out to solve the structure from powder diffraction data. For the hydrated structure, the peak cut-off was fixed to 10%, the map grid step to 0.1, and the lower threshold and upper limit for charge flipping to 0.1 and 18, respectively. For the anhydrous structure, the peak cut-off was fixed to 10%, the map grid step to 0.15, the lower threshold and upper limit for charge flipping to 0.2 and 20, respectively. After solving the structure, Rietveld refinement was carried out by refining the scale factor, the chebyschev background function, the unit cell parameters, the μstrain, and the atomic parameters in this order. Further details on the charge flipping algorithm may be found in reference [21]. XAS experiments were performed at Elettra–Sincrotrone Trieste (Italy), at the XAFS beamline [22]. The storage ring operated at 2.0 GeV in top-up mode with a typical current of 310 mA. XAS data were recorded at Fe and Cu K-edges by using ionization chambers filled with a mixture of Ar, N2, and He, in transmission mode. The energy was calibrated using internal references of iron and copper foil (the first inflection point of the XAS spectra were set to 7112 and 8979 eV, respectively, for iron and copper. Spectra at Fe and Cu K-edges were collected with a constant k-step of 0.03 Å−1 with 2 s/point acquisition time. Data were collected from 6950 to 8050 eV for the Fe K-edges and from 8760 to 9850 eV for the Cu K-edges. The energy of the synchrotron beam was selected by using a fixed exit monochromator equipped with a pair of Si(111) crystals. Harmonics rejection was performed by using the cut-off of the reflectivity of the platinum mirror placed at 3 mrad with respect to the beam upstream (Cu K-edge) or by detuning the second crystal of the monochromator by 30% of the maximum (Fe K-edge).PDF Image | Cross-Investigation on Copper Nitroprusside: Combining XRD and XAS
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