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Surface photovoltage microscopy for mapping charge separation on photocatalyst particles

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Abstract

Solar-driven photocatalytic reactions offer a promising route to clean and sustainable energy, and the spatial separation of photogenerated charges on the photocatalyst surface is the key to determining photocatalytic efficiency. However, probing the charge-separation properties of photocatalysts is a formidable challenge because of the spatially heterogeneous microstructures, complicated charge-separation mechanisms and lack of sensitivity for detecting the low density of separated photogenerated charges. Recently, we developed surface photovoltage microscopy (SPVM) with high spatial and energy resolution that enables the direct mapping of surface-charge distributions and quantitative assessment of the charge-separation properties of photocatalysts at the nanoscale, potentially providing unprecedented insights into photocatalytic charge-separation processes. Here, this protocol presents detailed procedures that enable researchers to construct the SPVM instruments by integrating Kelvin probe force microscopy with an illumination system and the modulated surface photovoltage (SPV) approach. It then describes in detail how to perform SPVM measurements on actual photocatalyst particles, including sample preparation, tuning of the microscope, adjustment of the illuminated light path, acquisition of SPVM images and measurements of spatially resolved modulated SPV signals. Moreover, the protocol also includes sophisticated data analysis that can guide non-experts in understanding the microscopic charge-separation mechanisms. The measurements are ordinarily performed on photocatalysts with a conducting substrate in gases or vacuum and can be completed in 15 h.

Key points

  • Probing the charge-separation properties of photocatalysts is a formidable challenge because of the spatially heterogeneous microstructures, complicated charge-separation mechanisms and low density of separated photogenerated charges.

  • Surface photovoltage microscopy as described in this protocol has sufficiently high spatial and energy resolution to enable direct mapping of surface-charge distributions and quantitative assessment of the charge-separation properties of individual photocatalyst particles.

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Fig. 1: Principle of SPV measurements with KPFM.
Fig. 2: Time limitations of SPVM and the alternative approaches.
Fig. 3: SPV measurements on the femtosecond–second timescales to track holistic charge-transfer processes on photocatalyst particles.
Fig. 4: Comparison between AM and FM mode KPFM for imaging of photocatalyst particles.
Fig. 5: Schematic diagram of the SPVM system.
Fig. 6: Schematic diagram of the light system assembly and its individual components.
Fig. 7: Comparison of modulated SPV signals with CPD signals in accuracy and sensitivity.
Fig. 8: Identification of multiple charge-separation processes.
Fig. 9: Focusing light on photocatalyst particles.
Fig. 10: Charge separation via asymmetric illumination in Cu2O photocatalyst particles as revealed by SPVM.
Fig. 11: Anisotropic charge separation via built-in electric field.
Fig. 12: Efficient charge separation via anisotropic defects.

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Data availability

All data generated or analyzed during this study are available at https://figshare.com/ (https://doi.org/10.6084/m9.figshare.24466933.v1) or from the corresponding author upon reasonable request.

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Acknowledgements

This work was financially supported by the National Natural Science Foundation of China (22372159, 22102173, 22088102 and 22325205), the Young Elite Scientist Sponsorship Program by CAST (YESS20220177), the National Program on Key Basic Research Project (2021YFA1500600 and 2021YFA1502300), CAS Projects for Young Scientists in Basic Research (YSBR-004) and Interdisciplinary Innovation Team (JCTD-2018-10) and the Dalian Institute of Chemical Physics Innovation Foundation (DICPSZ201801).

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  1. State Key Laboratory of Catalysis, Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian, China

    Ruotian Chen, Chenwei Ni, Jian Zhu, Fengtao Fan & Can Li

  2. University of Chinese Academy of Sciences, Beijing, China

    Chenwei Ni & Can Li

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C.L. conceived and proposed the project. R.C. and F.F. carried out the project. R.C. conceived the protocol, performed the experiments, analyzed the data and wrote and edited the manuscript. C.N. assisted in organizing procedures, J.Z. assisted in experimental setup and F.F. and C.L. revised the manuscript.

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Key references using this protocol

Chen, R. et al. Chem. Soc. Rev. 47, 8238–8262 (2018): https://doi.org/10.1039/C8CS00320C

Chen, R. et al. Nat. Energy 3, 655–663 (2018): https://doi.org/10.1038/s41560-018-0194-0

Chen, R. et al. Nature 610, 296–301 (2022): https://doi.org/10.1038/s41586-022-05183-1

Chen, R. et al. Nano Lett. 19, 426–432 (2019): https://doi.org/10.1021/acs.nanolett.8b04245

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Chen, R., Ni, C., Zhu, J. et al. Surface photovoltage microscopy for mapping charge separation on photocatalyst particles. Nat Protoc (2024). https://doi.org/10.1038/s41596-024-00992-2

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