In-Situ/Operando57Fe Mössbauer Spectroscopic Technique and Its Applications in NiFe-based Electrocatalysts for Oxygen Evolution Reaction

doi:10.13208/j.electrochem.210854

Abstract

Abstract:

The development of highly efficient and cost-effective electrocatalysts for the sluggish oxygen evolution reaction (OER) remains a significant barrier to establish effective utilization of renewable energy storage systems and water splitting to produce clean fuel. The current status of the research in developing OER catalysts shows that NiFe-based oxygen evolution catalysts (OECs) have been proven as excellent and remarkable candidates for this purpose. But it is critically important to understand the factors that influence their activity and underlying mechanism for the development of state-of-the-art OER catalysts. Therefore, the development of in-situ/operando characterizations is urgently required to detect key intermediates along with active sites and phases responsible for OER. ⁵⁷Fe Mössbauer spectroscopy is one of the appropriate and suitable techniques for determining the phase structure of catalysts under their electrochemical working conditions, identifying the active sites, clarifying the catalytic mechanisms, and determining the relationship between catalytic activity and the coordination structure of catalysts. In this tutorial review, we have discussed the current status of research on NiFe-based catalysts with particular attention to introduce in detail the knowhow about the development and utilization of in-situ/operando⁵⁷Fe Mössbauer-electrochemical spectroscopy for the study of OER mechanism. A brief overview using NiFe-(oxy)hydroxide catalysts, derived from ordered porous metal-organic framework (MOF) material NiFe-PBAs (Prussian blue analogues), as a typical model study case for the OER electrocatalyst and self-designed in-situ/operando⁵⁷Fe Mössbauer-electrochemical instrument, has been provided for the better understanding of readers. Moreover, using in-situ/operando⁵⁷Fe Mössbauer spectroscopy, the crucial role of Fe species during OER reaction has been explained very well.

Key words: oxygen evolution reaction, NiFe-(oxy)hydroxide electrocatalyst, NiFe Prussian blue analogue, in-situ/operando⁵⁷Fe Mössbauer spectroscopy, key intermediate detection

Jafar Hussain Shah, Qi-Xian Xie, Zhi-Chong Kuang, Ri-Le Ge, Wen-Hui Zhou, Duo-Rong Liu, Alexandre I. Rykov, Xu-Ning Li, Jing-Shan Luo, Jun-Hu Wang. In-Situ/Operando⁵⁷Fe Mössbauer Spectroscopic Technique and Its Applications in NiFe-based Electrocatalysts for Oxygen Evolution Reaction[J]. Journal of Electrochemistry, 2022, 28(3): 2108541.

Figures/Tables 18

References 76

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Sample	Valence/spin state	δ/Fe (mm·s^-1)	Δ (mm·s^-1)	Γ_exp(mm·s^-1)	A (%)
NiFe_0.11-Fe PBA	Fe^Ⅲ high spin	0.44	0.50	0.43	14
NiFe_0.11-Fe PBA	Fe^Ⅲ low spin	-0.17	0.50	0.38	86
NiFe_0.2-Fe PBA	Fe^Ⅲ high spin	0.40	0.65	0.38	19
NiFe_0.2-Fe PBA	Fe^Ⅲ low spin	-0.16	0.59	0.46	81
NiFe_0.25-Fe PBA	Fe^Ⅲ high spin	0.37	0.65	0.34	21
NiFe_0.25-Fe PBA	Fe^Ⅲ low spin	-0.15	0.62	0.45	79
NiFe_0.29-Fe PBA	Fe^Ⅲ high spin	0.37	0.64	0.36	24
NiFe_0.29-Fe PBA	Fe^Ⅲ low spin	-0.15	0.57	0.44	76

Sample	Valence/spin state	δ/Fe (mm·s^-1)	Δ (mm·s^-1)	Γ_exp (mm·s^-1)	A (%)
NiFe_0.11-O_xH_y	Fe³⁺ high spin	0.32	0.44	0.28	100
NiFe_0.2-O_xH_y	Fe³⁺ high spin	0.32	0.58	0.42	100
NiFe_0.25-O_xH_y	Fe³⁺ high spin	0.34	0.35	0.36	100
NiFe_0.29-O_xHy	Fe³⁺ high spin	0.32	0.43	0.33	100

This work^[65] (NiFe_0.2-O_xH_y)			Previous report^[47] (Layered 3:1 NiFe oxyhydroxide)
Potential (V vs. RHE)	Fe⁴⁺		Potential (V vs. RHE)	Fe⁴⁺
Potential (V vs. RHE)	Fe⁴⁺(%)	δ/Fe (mm·s^-1)	Potential (V vs. RHE)	Fe⁴⁺ (%)	δ/Fe (mm·s^-1)
1.32	0	-	-	-	-
1.37	2	-0.25	-	-	-
1.42 (around onset)	12	-0.24	1.49 (around onset)	0	-
1.47	23	-0.25	-	-	-
1.52	36	-0.24	-	-	-
1.57	40	-0.25	1.62	12	-0.27
-	-	-	1.76	21	-0.25

In-Situ/Operando⁵⁷Fe Mössbauer Spectroscopic Technique and Its Applications in NiFe-based Electrocatalysts for Oxygen Evolution Reaction

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