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The content of high-valent iron in-situ produced in the NiFe_0.2-O_xH_y electrocatalyst during the oxygen evolution reaction.
The in-situ/operando ⁵⁷Fe Mössbauer spectra of NiFe_0.2-O_xH_y collected at (A) the open circuit voltage, (B) 1.37 V, (C) 1.42 V, (D) 1.47 V, and (E) 1.57 V (vs. RHE). (F) Ex-situ ⁵⁷Fe Mössbauer spectrum of NiFe_0.2-O_xH_y collected after OER. The unit of ⁵⁷Fe Mössbauer parameter of isomer shift (δ) is mm·s^-1 relative to standard α-Fe foil. (G) The current-time curves at different applied potentials obtained during the in-situ/operando measurements. (H) Cyclic voltammogram without i_R correction of NiFe_0.2-O_xH_y recorded during the in-situ/operando measurements. (I) The content of Fe⁴⁺ and corresponding electric current determined at different applied potentials^[66]. Copyright 2021. ELSEVIER B.V. Reproduced with permission. (color on line)
(A) Cyclic voltammetric curves of NiFe_0.2-O_xH_y before (the black curves, α-phase Ni(OH)₂ structure) and after electrochemical activation (the red curves, γ-phase NiOOH structure). (B-C) ⁵⁷Fe Mössbauer spectra of NiFe_0.2-O_xH_y before and after electrochemical activation. (D) Raman spectra of NiFe_0.2-O_xH_y before (black) and after (red) applying anodic potential. (E) Operando Raman spectra of NiFe_0.2-O_xH_y collected at different applied potentials (V vs. RHE). (F) The OER polarization curves with i_R correction. (G) Overpotentials at 10 mA·cm^-2. (H) Tafel plots of NiFe_m-O_xH_y with different molar ratios of Fe/Ni and commercial RuO₂. (I) Chronopotentiometric curves of NiFe_0.2-O_xH_y on Ni foam with different catalyst loadings at a constant current density of 100 mA·cm^-2 for 100 h. The inset shows the chronopotentiometric curve of NiFe_0.2-O_xH_y at a constant current density of 10 mA·cm^-2[66]. Copyright 2021. ELSEVIER B.V. Reproduced with permission. (color on line)
Ex-situ ⁵⁷Fe Mössbauer spectral parameters of NiFe_m-O_xH_y at room temperature
Ex-situ ⁵⁷Fe Mössbauer spectral parameters of NiFe_m-Fe PBAs at room temperature
(A-D) Ex-situ ⁵⁷Fe Mössbauer analysis of NiFe_m-Fe PBAs doped with different ratios of Ni:Fe. (E-H) Ex-situ ⁵⁷Fe Mössbauer analysis of NiFe_m-O_xH_y derived from the precursors NiFe_m-Fe PBAs by topotactic transformation. (color on line)
(A) Linear sweep voltammetric results of NiFe-PBAs/CNTs with varying amount of CNTs. (B) Tafel slopes for NiFe-PBAs/CNTs. (C) XRD analysis showing the structures of NiFe-PBAs/CNTs, carbon paper, NiFe-PBAs/CNTs/carbon paper, and NiFe-PBAs/CNTs/carbon paper after activation through cyclic voltammetry. (D) Ex-situ ⁵⁷Fe Mössbauer spectroscopic analysis of NiFe-PBAs/CNTs before and after CV activation. (E) Raman spectra for NiFe-PBAs/CNTs before and after CV activation. (F) In-situ/operando Raman spectroscopic analysis for NiFe-PBAs/CNTs at different applied potentials. (color on line)
(A) A schematic diagram of self-designed in-situ/operando ⁵⁷Fe and ¹¹⁹Sn Mössbauer electrochemical reaction cell. (B) A schematic illustration of multiple working electrodes parallel arrangement inside the reactor. (color on line)
(A) Fabricated electrodes for in-situ/operando Mössbauer-electrochemical test. (B) A front view of self-designed Mössbauer-electrochemical reaction cell connected with electrochemical station. (C) In-situ/operando Mössbauer-electrochemical cell placed inside the Mössbauer instrument ready for coinstantaneous OER reaction and Mössbauer measurement. (D) The schematic illustration of in-situ/operando electrochemical ⁵⁷Fe and ¹¹⁹Sn Mössbauer setup for electrochemical OER characterizations^[66]. Copyright 2021. ELSEVIER B.V. Reproduced with permission. (color on line)
Different line shapes employed for approximation of practically measured ⁵⁷Fe Mössbauer spectra. (color on line)
Schematic illustration of (upper part) configuring a Mössbauer spectrometer copied with permission from webpage: http://www.wissel-instruments.de/ and (lower part) Operational modes of Mössbauer spectroscopy for observing a spectrum: Transmission mode (right) and backscattering mode (left, CEMS measurement). (color on line)
(A) Schematic illustration for emission of specific energy γ-rays from the excited state of nucleus in the Mössbauer source and recoilless γ-rays resonant absorption of the same nucleus in the ground state in the absorber (sample). (B) Nuclear energy levels splitting in case of a transition between I_g = 1/2 and I_e = 3/2 like that of ⁵⁷Fe due to electric monopole interaction, or electric quadrupole interaction or magnetic hyperfine interaction, and the corresponding ⁵⁷Fe Mössbauer spectra.
Selected in-situ/operando spectroscopic characterization techniques for being available to capture the NiFe-based OER electrocatalytic intermediate species, investigating the OER pathways and mechanism^[54]. Copyright 2021. Elsevier Inc. Reproduced with permission. (color on line)
CVs of NiFe layered oxyhydroxide (blue) and hydrous Fe oxide (green) electrocatalysts used for the in-situ/operando experiments with ⁵⁷Fe Mössbauer spectra collected at open circuit potential (gray), 1.49 V(purple), 1.62 V(yellow), and 1.76 V(red) vs. RHE. CV data were recorded in the Mössbauer-electrochemical cell with a scan rate of 25 mV·s^-1 prior to Mössbauer measurements^[47]. Copyright 2015. American Chemical Society. Reproduced with permission. (color on line)
In-situ/operando XAS of the NiFe OER catalysts with varying catalyst composition Ni_100-_xFe_x: (A) Fe K-edges and (B) Ni K-edges^[37]. Copyright 2016 American Chemical Society. Reproduced with permission. (color on line)
Cyclic voltammograms were taken during the aging of films in various purities of KOH. A total of 13 CV scans are shown for each sample: one for the initial as-deposited film (the dark purple), and one additional scan after each 5 min aging period up to a total of 1 hour of aging (the dark red). The changes in the anodic and cathodic peak positions (ΔE_p,a and ΔE_p,c) are labeled for each set of CVs. (ΔE_p,a value is shown for the Ni_0.75Fe_0.25(OH)₂, as the oxidation peak is partially obscured by the OER current.)^[36] Copyright 2014 American Chemical Society. Reproduced with permission. (color on line)
Steady-state effective conductivity of NiO_xH_y on an interdigitated array (IDA) electrode as a function of Fe incorpo-ration from 1 mmol·L^-1 Fe(NO₃)₃ in a 1 mol·L^-1 aqueous KOH solution^[34]. Copyright 2017 American Chemical Society. Reproduced with permission. （color on line）
(A) Schematic of the electrochemical water splitting; (B) The reported OER mechanism for alkaline conditions^[11]. Copyright@The Royal Society of Chemistry 2019. Reproduced with permission. (color on line)
(A) Specific recognition molecules for K⁺, Na⁺, pH, and Ca²⁺. (B) Schematic structures of 5-channel ion selective microelectrode arrays (5-ISMEA) and 8-channel M-ISMEA (K-ISMEA, Ca-ISMEA, Na-ISMEA or H-ISMEA). (C) LFP signals recorded in a live rat brain upon seizure, and the developed ECPM for real-time mapping and simultaneous quantification of multi-ions in the brain of a freely moving rat. (D) Potential responses of 5-ISMEA toward KCl, NaCl, CaCl₂, and HCl in 0.1 mol·L^-1 Tris-buffer. (E) 3D surface plots of potential separation (ΔEISE) or K⁺, Na⁺, Ca²⁺, pH responses of KISME, Na-ISME, Ca-ISME, and H-ISME as a function of one kind of ion and the other three ions. Reproduced with permission of Ref. 25. Copyright 2020 Angewandte Chemie-International Edition. (color on line)
(A) Illustration for multi-fiber microarray and measurements in the mouse brain. (B) SEM images of DPACE (top) and EDACE (bottom). (C) EDX analysis images of the selected areas of Au (yellow) and GO (blue) on DPACE (top) and EDACE (bottom). (D) Fluorescence images of DPACE and EDACE after immersed in 20 mg·mL^-1 FITC-BSA solution for 2 h. (E) Molecular structures of METH (left), M18C6 (middle) and MBAPTA (right), and the modification of three ligands onto electrode surfaces. (F) The potential changes (vs. Ag/AgCl) obtained at METH-E (left), M18C6-E (middle), and MBAPTA-E (right) with continuously increasing concentration of Ca²⁺ and decreasing concentration of Ca²⁺ in aCSF. Reproduced with permission of Ref. 26. Copyright 2021 Angewandte Chemie-International Edition. (color on line)

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