Powder x-ray diffraction patterns were measured for the samples filled inside a capillary with an inner diameter of 200 μm using a synchrotron x-ray source (λ = 0.65296 Å) in the BL15XU beam line at SPring-8, Harima, Japan 30. SeM-eDS measurements. A small piece of the produced powder was suspended in ethanol by ultrasonication until a homogeneous suspension was obtained. The suspension was dropped onto an aluminium sample holder, dried, and examined by scanning electron microscopy (SEM) with electron dispersion spectroscopy (EDS) operated at 15 kV (JSM-7600F, JEOL). Mössbauer measurements. We measured the 57 Fe Mössbauer spectra using the constant acceleration method, using a 57 Co(Rh) source and an α-Fe a reference. γ-Ray radiation was monitored with a multi-channel analyser (MCA-7700, Seiko EG&G) using 512 channels for each spectrum. The obtained spectra were analysed by Lorentzian fitting using Mösswinn 3.0i XP. Magnetic measurements. We measured the magnetic properties using a conventional superconducting quantum interference device (SQUID) magnetometer (MPMS-XL, Quantum Design) under a magnetic field of up to 50 kOe in the temperature range from 5 to 300 K for dc-magnetization.
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