In this mini-review of our research group’s activity, the application of ⁵⁷Fe Mössbauer spectroscopy in studies of electronic structure, coordination environment, and magnetic interactions in an interesting series of Fe(II/III) compounds selected is discussed. We selected two prominent phenomena that arose during investigations of selected groups of compounds carried out at different periods of time: (1) very high magnetic hyperfine fields observed at low temperatures; (2) changes in the oxidation state of the central iron atom of complexes in the solid state during interactions with gaseous O₂/H₂O mixtures, resulting in spin crossover (SCO).

A new and simple method is developed to synthesize carbon microspheres decorated with iron sulfide nanoparticles for mercury ion removal from water. The synthesis is based on carbonizing polystyrene–divinylbenzene-based and iron(III) sulfate-loaded cation exchange resins between 500 and 1000 °C. The phase composition, surface area, and morphology of these materials are characterized by various spectroscopic and diffraction techniques, including Mössbauer spectroscopy, powder X-ray diffraction, Raman and scanning electron microscopy, and BET analysis. Pyrrhotite is found to be the dominant iron-containing phase. The adsorption performance of microspheres for mercury ion removal from water is studied as a function of adsorbent load and contact time at pH 6.5 using a solution of 40 mg dm⁻³mercury ion. Pyrrhotite nanoparticles played a key role in mercury ion removal amounting to 70–90% of the extracted amount. A high adsorption capacity of 104 mg of mercury/g of adsorbent at an adsorbent load of 0.33 g dm⁻³is achieved, and the removal kinetics could be well fitted with a pseudo-second-order kinetic model, indicating chemical sorption. The synthetic method is easy to scale up for large-scale production and materials are easy to handle, which is significant for large-scale environmental applications.

In this paper, a relationship between the structure and the electrical properties of a nanocrystalline composite ceramics xNa₂O·(100 − x)V₂O₅ with ‘x’ of 5, 15, 25, 35, and 45 mol%, abbreviated as xNV, was investigated by X-ray diffractometry (XRD), X-ray absorption spectroscopy (XAS), Cyclic Voltammetry (CV), Electrochemical impedance spectroscopy (EIS), and cathode active performance in Na-ion battery (SIB). For the expected sodium vanadium bronzes (Na_xV₂O₅) precipitation, the preparation of xNV was performed by keeping the system in the molten state at 1200 °C for one hour, followed by a temperature decrease in the electric furnace to room temperature at a cooling rate of 10 °C min⁻¹. XRD patterns of the 15NV ceramic exhibited the formation of Na_0.33V₂O₅ and NaV₃O₈ crystalline phases. Moreover, the V K-edge XANES showed that the absorption edge energy of ceramics 15NV recorded at 5479 eV is smaller than that of V₂O₅ at 5481 eV, evidently indicating a partial reduction from V⁵⁺ to V⁴⁺ due to the precipitation of Na_0.33V₂O₅. In the cyclic voltammetry, reduction peaks of 15NV were observed at 1.12, 1.78 V, and 2.69 V, while the oxidation peak showed up only at 2.36 V. The values of the reduction peaks were related to the NaV₃O₈ crystalline phase. Moreover, the diffusion coefficient of Na⁺ (D_Na⁺) gradually decreased from 8.28 × 10⁻¹¹ cm² s⁻¹ to 1.23 × 10⁻¹² cm² s⁻¹ with increasing Na₂O content (x) from 5 to 45 mol%. In the evaluation of the active cathode performance of xNV in SIB, ceramics 15NV showed the highest discharge capacity 203 mAh g⁻¹ at a current rate of 50 mA g⁻¹. In the wider voltage range from 0.8 to 3.6 V, the capacity retention was maintained at 50% after 30 cycles, while it was significantly improved to 90% in the narrower voltage range from 1.8 to 4.0 V, although the initial capacity decreased to 56 mAh g⁻¹. It is concluded that the precipitation of the Na_0.33V₂O₅ phase improved the structural and electrical properties of 15NV, which provides a high capacity for the Na-ion battery when incorporated as a cathode active material.

The present study investigates the relationship between the local structure, photocatalytic ability, and cathode performances in sodium-ion batteries (SIBs) and lithium-ion batteries (LIBs) using Ni-substituted goethite nanoparticles (Ni_xFe_1−xOOH NPs) with a range of ‘x’ values from 0 to 0.5. The structural characterization was performed applying various techniques, including X-ray diffractometry (XRD); thermogravimetry differential thermal analysis (TG-DTA); Fourier transform infrared spectroscopy (FT-IR); X-ray absorption spectroscopy (XANES/EXAFS), both measured at room temperature (RT); ⁵⁷Fe Mössbauer spectroscopy recorded at RT and low temperatures (LT) from 20 K to 300 K; Brunauer–Emmett–Teller surface area measurement (BET), and diffuse reflectance spectroscopy (DRS). In addition, the electrical properties of Ni_xFe_1−xOOH NPs were evaluated by solid-state impedance spectroscopy (SS-IS). XRD showed the presence of goethite as the only crystalline phase in prepared samples with x ≤ 0.20, and goethite and α-Ni(OH)₂ in the samples with x > 0.20. The sample with x = 0.10 (Ni10) showed the highest photo-Fenton ability with a first-order rate constant value (k) of 15.8 × 10⁻³ min⁻¹. The ⁵⁷Fe Mössbauer spectrum of Ni0, measured at RT, displayed a sextet corresponding to goethite, with an isomer shift (δ) of 0.36 mm s⁻¹ and a hyperfine magnetic distribution (B_hf) of 32.95 T. Moreover, the DC conductivity decreased from 5.52 × 10⁻¹⁰ to 5.30 × 10⁻¹² (Ω cm)^–1 with ‘x’ increasing from 0.10 to 0.50. Ni20 showed the highest initial discharge capacity of 223 mAh g⁻¹, attributed to its largest specific surface area of 174.0 m² g⁻¹. In conclusion, Ni_xFe_1−xOOH NPs can be effectively utilized as visible-light-activated catalysts and active cathode materials in secondary batteries.