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In-situ monitoring of dynamic behavior of catalyst materials and reaction intermediates in semiconductor catalytic processes

Zhen Fang1, 2, Yao Liu3, Chengyi Song1, 2, Peng Tao1, 2, Wen Shang1, 2, Tao Deng1, 2, Xiaoqin Zeng3, and Jianbo Wu1, 2, 4, 5,

+ Author Affiliations

 Corresponding author: Xiaoqin Zeng, xqzeng@sjtu.edu.cn; Jianbo Wu, jianbowu@sjtu.edu.cn

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Abstract: Semiconductor photocatalysis, as a key part of solar energy utilization, has far-reaching implications for industrial, agricultural, and commercial development. Lack of understanding of the catalyst evolution and the reaction mechanism is a critical obstacle for designing efficient and stable photocatalysts. This review summarizes the recent progress of in-situ exploring the dynamic behavior of catalyst materials and reaction intermediates. Semiconductor photocatalytic processes and two major classes of in-situ techniques that include microscopic imaging and spectroscopic characterization are presented. Finally, problems and challenges in in-situ characterization are proposed, geared toward developing more advanced in-situ techniques and monitoring more accurate and realistic reaction processes, to guide designing advanced photocatalysts.

Key words: in-situsemiconductor photocatalystmaterials evolutionreaction intermediate



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Fig. 1.  (Color online) In-situ characterization of semiconducting photocatalysts for material research and mechanism disclosure in solar energy conversion and the storage process.

Fig. 2.  (Color online) Energy band diagram and electron distribution of three typical types of semiconductors, including (a) intrinsic type, (b) negative-type, and (c) positive-type. (d) Mechanism displays of semiconductor photocatalysis.

Fig. 3.  (Color online) Schematic diagram of the interaction between particles (electrons and photons) and materials.

Fig. 4.  (Color online) (a) In-situ STM observation of oxygen vacancies dynamic changes on TiO2(110) surface. (b) In-situ XPS, in-situ EPR, in-situ XAS (XANES) and in-situ EXAFS spectra in R space of WO3-600. (c) Series of in-situ TEM images of a CeO2 nanoparticle. (d) In-situ TEM images of atom mobility on CeO2 surface at {100} facet in high vacuum, oxygen, and carbon dioxide atmospheres. Modified with permission from (a) Ref. [32] Copyright 2018 American Chemical Society, (b) Ref. [33] Copyright 2019 WILEY-VCH Verlag GmbH & Co. KGaA, (c) Ref. [35] Copyright 2017 American Chemical Society, (d) Ref. [36] Copyright 2011 WILEY-VCH Verlag GmbH & Co. KGaA.

Fig. 5.  (Color online) (a) In-situ TEM images of TiO2 under water vapor conditions, with (b) EELS spectra and (c) XPS spectra of TiO2 particles. In-situ TEM study of TiO2 photocatalytic water splitting under UV light: (d) formation and evolution of bubbles, (e) magnified views of the surface shell on TiO2, (f) schematic diagrams of fluidic TEM holder with in-situ UV illumination, (g) surface shell thickness on TiO2 under UV illumination and (h) EELS spectra of the TiO2. (i) HRTEM images of Cu2O samples irradiated for 1, 2, and 3 h, as well as schematic diagrams of Cu2O structure change during irradiation. Modified with permission from (a), (b) and (c) Ref. [38] Copyright 2013 American Chemical Society, (d), (e), (f), (g) and (h) Ref. [39] Copyright 2018 Springer Nature, (i) Ref. [40] Copyright 2020 Elsevier Ltd.

Fig. 6.  (Color online) (a) Schematic diagram of water reduction in Au-TiO2 with UV- (right) and visible-light (left) driven. (b) In-situ EPR spectra of TiO2 and Au-TiO2. (c) In-situ XAS spectra of THMSs and Au THMSs. (d) Schematic illustration of the electron transfer mechanism between TiO2/ZnIn2S4 S-scheme heterojunction. (e) In-situ XPS spectra of TiO2, ZnIn2S4, and TiO2/ZnIn2S4. (f) In-situ TEM observations about evolution and dynamic structural changes of the overlayer in a strong metal-support interaction. (g) Time-series in-situ ETEM image of Pt-loaded CeO2. Modified with permission from (a) and (b) Ref. [43] Copyright 2013 Wiley-VCH Verlag GmbH & Co. KGaA, (c) Ref. [44] Copyright 2018 American Chemical Society, (d) and (e) Ref. [52] Copyright 2021 Wiley-VCH GmbH, (f) Ref. [53] Copyright 2021 Springer Nature, (g) Ref. [54] Copyright 2020 Springer Nature.

Fig. 7.  (Color online) In-situ characterization of reaction intermediates in the photocatalytic HER and OER processes. (a) Mechanism scheme of HER and OER. (b) LSV curve (left) and (c) operando Raman spectra (right) of MoS0.9Se1.1. (d) Schematic illustration of the HER process in MoS2xSe2(1–x). (e) In-situ DRIFT spectra of H2O on the ZnIn2S4@MoS2 with 2 h H2O-saturated flow under He and (f) with a 2 h irradiation time under Xe lamp, and (g) proposed reaction pathway for the HER process over the ZnIn2S4@MoS2. In-situ FTIR spectra of the HER process on ReS2/CdS with two different sacrificial agents, (h) Na2S-Na2SO3 and (i) lactic acid. Modified with permission from (b), (c) and (d) Ref. [64] Copyright 2020 Wiley-VCH Verlag GmbH & Co. KGaA, (e), (f) and (g) Ref. [65] Copyright 2021 Elsevier Ltd., (h) and (i) Ref. [66] Copyright 2019 Elsevier Ltd.

Fig. 8.  (Color online) In-situ characterization of reaction intermediates in the photocatalytic CO2 conversion processes. (a) Mechanism scheme of CO2 conversion. (b) In-situ FTIR spectra of CO2 adsorbed on the BiOBr layers with oxygen vacancy in the presence of H2O vapor. (c) Schematic illustration for CO2 photoconversion into CO over the oxygen-vacancy BiOBr. (d) In-situ DRIFTS spectra for the conversion process of CO2 in the presence of CH3OH under Xe lamp for oxygen vacancy-rich-Bi2O3 nanosheets. (e) Schematic illustration for CO2 photofixation to long-chain chemicals. (f) In-situ DRIFTS spectra of CO2 reduction reaction and (g) possible photocatalytic pathways over the TiO2@ZnIn2S4. In-situ FTIR spectra of atmospheric 0.03 vol % CO2/Ar photothermal reduction over the oxygen vacancy-rich Zn2GeO4 nanobelts at (h) 293 K and (i) 348 K. (j) Function mechanism of photoinduced heat during CO2 photoreduction to CH3COOH. Modified with permission from (b) and (c) Ref. [80] Copyright 2021 Wiley-VCH GmbH, (d) and (e) Ref. [81] Copyright 2019 Springer Nature, (f) and (g) Ref. [52] Copyright 2018 Wiley-VCH Verlag GmbH & Co. KGaA, (h), (i) and (j) Ref. [82] Copyright 2021 American Chemical Society.

Fig. 9.  (Color online) In-situ characterization of reaction intermediates in the N2 photofixation process. (a) Mechanism scheme of N2 fixation. In-situ IR spectra of Bi5O7Br-40 in the process of (b) N2 adsorption from 0 to 40 min in the dark, (c) afterward receive visible light illumination, (d) then visible light illumination lasts 35 min, and (e) finally the visible light illumination is turned off. (f) In-situ DRFTIRS spectra were obtained and (g) a reaction pathway of N2 photofixation over the Bi5O7Br nanotubes. Modified with permission from (b), (c), (d) and (e) Ref. [94] Copyright 2020 American Chemical Society, (f) and (g) Ref. [95] Copyright 2020 American Chemical Society.

Fig. 10.  (Color online) In-situ characterization of reaction intermediates in other catalytic processes. In-situ FTIR spectra of (a) TiO2-OV and (b) TiO2. (c) Selective removal mechanism during the NO removal process over the TiO2-OV and TiO2. (d) In-situ FTIR spectra and (e) NO removal mechanism of Bi0OVs-(BiO)2CO3. Modified with permission from (a), (b) and (c) Ref. [98] Copyright 2019 American Chemical Society, (d) and (e) Ref. [97] Copyright 2019 Elsevier Ltd.

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    Received: 02 December 2021 Revised: 12 January 2022 Online: Accepted Manuscript: 14 March 2022Uncorrected proof: 15 March 2022Published: 18 April 2022

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      Zhen Fang, Yao Liu, Chengyi Song, Peng Tao, Wen Shang, Tao Deng, Xiaoqin Zeng, Jianbo Wu. In-situ monitoring of dynamic behavior of catalyst materials and reaction intermediates in semiconductor catalytic processes[J]. Journal of Semiconductors, 2022, 43(4): 041104. doi: 10.1088/1674-4926/43/4/041104 Z Fang, Y Liu, C Y Song, P Tao, W Shang, T Deng, X Q Zeng, J B Wu. In-situ monitoring of dynamic behavior of catalyst materials and reaction intermediates in semiconductor catalytic processes[J]. J. Semicond, 2022, 43(4): 041104. doi: 10.1088/1674-4926/43/4/041104Export: BibTex EndNote
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      Zhen Fang, Yao Liu, Chengyi Song, Peng Tao, Wen Shang, Tao Deng, Xiaoqin Zeng, Jianbo Wu. In-situ monitoring of dynamic behavior of catalyst materials and reaction intermediates in semiconductor catalytic processes[J]. Journal of Semiconductors, 2022, 43(4): 041104. doi: 10.1088/1674-4926/43/4/041104

      Z Fang, Y Liu, C Y Song, P Tao, W Shang, T Deng, X Q Zeng, J B Wu. In-situ monitoring of dynamic behavior of catalyst materials and reaction intermediates in semiconductor catalytic processes[J]. J. Semicond, 2022, 43(4): 041104. doi: 10.1088/1674-4926/43/4/041104
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      In-situ monitoring of dynamic behavior of catalyst materials and reaction intermediates in semiconductor catalytic processes

      doi: 10.1088/1674-4926/43/4/041104
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      • Zhen Fang:received his MS from Wuhan University of Technology in 2021. Now he is a PhD candidate student at Shanghai Jiao Tong University under the supervision of Prof. Jianbo Wu. His research focuses on in-situ TEM characterization, and platinum-based electrocatalyst
      • Yao Liu:received her MS from Hunan University in 2021. Now she is a PhD candidate student at Shanghai Jiao Tong University under the supervision of Prof. Xiaoqin Zeng. Her research focuses on in-situ corrosion of metals and alloys
      • Xiaoqin Zeng:received his PhD degree from Shanghai Jiao Tong University in 2001, and now he is a professor in the School of Materials Science and Engineering at Shanghai Jiao Tong University. He was a recipient of the National Science Foundation for outstanding young scholars. His main research interests include strengthening theory and method of alloys and design and preparation of advanced Mg alloys
      • Jianbo Wu:is a professor in the School of Materials Science and Engineering at Shanghai Jiao Tong University. He received his PhD degree in Chemical Engineering from University of Rochester in 2012, his MS degree in 2007 and BE degree in 2005 both in Materials Science and Engineering from Zhejiang University. He received postdoctoral training in the Department of Materials Science and Engineering at the University of Illinois at Urbana-Champaign. His current research focuses on facet and composition controlled nanocrystals, fuel cell electrocatalysts, functional materials for energy and environmental applications, and in situ TEM characterization
      • Corresponding author: xqzeng@sjtu.edu.cnjianbowu@sjtu.edu.cn
      • Received Date: 2021-12-02
      • Accepted Date: 2022-03-11
      • Revised Date: 2022-01-12
      • Available Online: 2022-03-25

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