Progress of In situ Raman Study on the Dynamic Structure Performance Correlation of Water Splitting Catalysts

doi:10.19894/j.issn.1000-0518.220001

Chinese Journal of Applied Chemistry ›› 2022, Vol. 39 ›› Issue (4): 528-539.DOI: 10.19894/j.issn.1000-0518.220001

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Progress of In situ Raman Study on the Dynamic Structure Performance Correlation of Water Splitting Catalysts

Hui-Bing TAO¹, Zhen TIAN², Yong XIE², Yu SUN², Li WANG¹(), Zhuo KANG²(), Yue ZHANG²

^1.Academy for Advanced Interdisciplinary Science and Technology，University of Science and Technology Beijing，Beijing 100083，China
^2.School of Materials Science and Engineering，Academy for Advanced Interdisciplinary Science and Technology，State Key Laboratory for Advanced Metals and Materials，University of Science and Technology Beijing，Beijing 100083，China

Received:2022-01-04 Accepted:2022-02-21 Published:2022-04-01 Online:2022-04-19
Contact: Li WANG,Zhuo KANG
Supported by:
the National Key Research and Development Program of China(2018YFA0703503);the Overseas Expertise Introduction Projects for Discipline Innovation(B14003);the National Natural Science Foundation of China(51991340)

Abstract

Abstract:

Electrolyzing water to hydrogen supported by renewable energy is pivotal for achieving the goal of carbon neutrality and the development of a sustainable society in the future. However， catalytic materials often undergo complex structural evolution during the service process of electrolyzing water， which poses a great challenge to in-depth understand the reaction mechanism of the process of electrolyzing water and precise design of high-efficiency catalytic materials. The real-time monitoring of the dynamic evolution process of the catalytic material structure through in situ electrochemical Raman characterization technology is the key to reveal the dynamic structure-activity correlation of the electrolyzed water material as well as the mechanism of the catalytic reaction. This review introduces the basic principles of in situ electrochemical Raman characterization technology， focusing on the latest developments in the phase structure evolution of catalytic materials， surface active sites and the behavior of interfacial water molecules， and considers the change law between the structure and performance evolution for electrolytic water catalytic materials in service， which provides a technical basis for the accurate construction of dynamic structure-activity correlation in the full life cycle of catalytic materials. Lastly， the problems and challenges of in situ electrochemical Raman characterization technology in the application toward electrolytic water are analyzed and summarized， prospecting the future development of advanced in situ electrochemical Raman technology.

Key words: Water electrolysis materials, In situ electrochemical Raman spectroscopy, Phase structure evolution, Surface active sites, Interface water molecular behavior

CLC Number:

O657.3

Hui-Bing TAO, Zhen TIAN, Yong XIE, Yu SUN, Li WANG, Zhuo KANG, Yue ZHANG. Progress of In situ Raman Study on the Dynamic Structure Performance Correlation of Water Splitting Catalysts[J]. Chinese Journal of Applied Chemistry, 2022, 39(4): 528-539.

Figures/Tables 6

Fig.1 Schematic diagram of the setup of electrochemical/Raman spectroscopy［27］

Fig.2 （A） In situ Raman spectra of La1-x Ce x NiO3 （x=0， 0.05， 0.1 and 0.15） during the OER process （1.0~1.7 V vs RHE）. （B） The surface reconstruction process of La1-x Ce x NiO3 to active structure of NiOOH by the A-site management of Ce substitution strategy. The correlation between surface reconstruction potential and the corresponding onset potential for OER. （C） The correlation between surface reconstruction potential and the corresponding onset potential for OER［33］. （D） In situ Raman spectra collected during the OER process in 0.1 mol/L KOH within a low-wavenumber region of 200~2000 cm-1［42］

Fig.3 （A） In situ Raman spectra of the Ni1-x Fe x S2 （x=0， 0.1， 0.2， 0.25 and 0.33） samples at the potentials of 0.4 to -0.25 V versus the reversible hydrogen electrode （vs. RHE） in 1 mol/L KOH. （B） Elemental composition of post-electrolysis Ni0.8Fe0.2S2 determined from EDS at a series of spots along a line from the crystallite edge to the bulk reveals the variation in Ni（Fe）∶S composition across the crystallite. （C） The surface reconstruction potential threshold range for the Ni1-x Fe x S2 （x=0~0.33） samples， and the corresponding onset potentials of hydrogen evolution are plotted to show the dynamic correlation of structure-activity. The red diamond dots represent the final potential of the existence of Raman peaks for the Ni1-x Fe x S2 structures， and the blue diamond dots stand for the potential of emerging Ni3S2 Raman peaks［44］. （D） Potential-dependent in situ Raman spectra of metal Ni with 0.1 mol/L MoO42-［45］

Fig.4 In?situ Raman spectrum of 18O labeled （A） Ni LDHs and （B） NiFe LDHs measured at 1.65 V （vs. RHE） in 0.1 mol/L KOH. The left column and right column represent the NiOOH and NiOO species， respectively. （C） Participation of lattice oxygen in Ni and NiCo LDHs. （D） Nonparticipation of lattice oxygen on NiFe LDH. M=Ni or Co［50］

Fig.5 （A） and （B） in situ Raman spectra of Pt-WO3 from 0.4 to -0.1 V［54］. （C） In situ Raman spectrum of cathodically deposited MoSx at different cathodic potential in 1 mol/L HClO4［59］. （D） In situ Raman spectra of the sample MoS0.9Se1.1 at voltages of 0.05， 0.00， -0.05， -0.10 and -0.15 V［60］ respectively. （E） In situ electrochemical surface-enhanced Raman spectroscopy （EC-SERS） of HER on Ag@MoS2 with size of （23.4 ± 3.8） nm in 0.5 mol/L H2SO4 electrolyte. （F） LSV curves for HER measured on the commercial Pt/C， Ag nanocrystals， MoS2 nanosheets， and Ag@MoS2 with different sizes［61］

Fig.6 （A） In situ Raman spectra of interfacial water on a Pd （111） electrode in a 0.1 mol/L NaClO4 solution （pH=11）. Gaussian fits of three O—H stretching modes are shown in blue， orange and red， respectively. c.p.s.， counts per second. （B） Schematic showing interfacial water dissociation on a Pd （111） surface （Au （111） coated with Pd monolayer）［21］. （C） In situ electrochemical Raman spectra at the Acid-PtNi1.5 surface in 0.1 mol/L NaOH［66］

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Progress of In situ Raman Study on the Dynamic Structure Performance Correlation of Water Splitting Catalysts

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