Direct Observation of Structural Evolution of Metal Chalcogenide in Electrocatalytic Water Oxidation

Fan, Ke; Zou, Haiyuan; Lu, Yue; Chen, Hong; Li, Fusheng; Liu, Jinxuan; Sun, Licheng; Tong, Lianpeng; Toney, Michael F.; Sui, Manling; Yu, Jiaguo

doi:10.1021/acsnano.8b06312

Title: Direct Observation of Structural Evolution of Metal Chalcogenide in Electrocatalytic Water Oxidation

Journal Article · Mon Dec 03 00:00:00 EST 2018 · ACS Nano

DOI:https://doi.org/10.1021/acsnano.8b06312· OSTI ID:1493412

^[1]; Zou, Haiyuan ^[1];

^[2];

^[3]; Li, Fusheng ^[4];

^[4];

^[5]; Tong, Lianpeng ^[6];

^[3];

^[2];

^[1]

Wuhan University of Technology (China)
Beijing University of Technology (China)
SLAC National Accelerator Lab., Menlo Park, CA (United States)
Dalian University of Technology (China)
Dalian University of Technology (China); KTH Royal Institute of Technology, Stockholm (Sweden)
Guangzhou University (China)

As one of the most remarkable oxygen evolution reaction (OER) electrocatalysts, metal chalcogenides have been intensively reported during the past few decades because of their high OER activities. It has been reported that electron-chemical conversion of metal chalcogenides into oxides/hydroxides would take place after the OER. However, the transition mechanism of such unstable structures, as well as the real active sites and catalytic activity during the OER for these electrocatalysts, has not been understood yet; therefore a direct observation for the electrocatalytic water oxidation process, especially at nano or even angstrom scale, is urgently needed. In this work, by employing advanced Cs-corrected transmission electron microscopy (TEM), a step by step oxidational evolution of amorphous electrocatalyst CoS_x into crystallized CoOOH in the OER has been in situ captured: irreversible conversion of CoS_x to crystallized CoOOH is initiated on the surface of the electrocatalysts with a morphology change via Co(OH)₂ intermediate during the OER measurement, where CoOOH is confirmed as the real active species. Besides, this transition process has also been confirmed by multiple applications of X-ray photoelectron spectroscopy (XPS), in situ Fourier-transform infrared spectroscopy (FTIR), and other ex situ technologies. Moreover, on the basis of this discovery, a high-efficiency electrocatalyst of a nitrogen-doped graphene foam (NGF) coated by CoS_x has been explored through a thorough structure transformation of CoOOH. In conclusion, we believe this in situ and in-depth observation of structural evolution in the OER measurement can provide insights into the fundamental understanding of the mechanism for the OER catalysts, thus enabling the more rational design of low-cost and high-efficient electrocatalysts for water splitting.

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Research Organization:: SLAC National Accelerator Lab., Menlo Park, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC02-76SF00515; WUT: 2017 IVA 092; 2015CFA001; 51772234; 11704015; 21433007; 21573170; 51320105001; 2017-ZD-4

OSTI ID:: 1493412

Journal Information:: ACS Nano, Vol. 12, Issue 12; ISSN 1936-0851

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 256 works

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cobalt chalcogenide
in situ TEM
structural evolution
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XPS

Title: Direct Observation of Structural Evolution of Metal Chalcogenide in Electrocatalytic Water Oxidation

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