Water oxidation sites located at the interface of Pt/SrTiO3 for photocatalytic overall water splitting

doi:10.1016/S1872-2067(21)64048-2

Abstract

Abstract:

When a proton reduction cocatalyst is loaded on an n-type semiconductor for photocatalytic overall water splitting (POWS), the location of water oxidation sites is generally considered at the surface of the semiconductor due to upward band-bending of n-type semiconductor which may ease the transfer of the photogenerated holes to the surface. However, this is not the case for Pt/SrTiO₃, a model semiconductor based photocatalyst for POWS. It was found that the photogenerated holes are more readily accumulated at the interface between Pt cocatalyst and SrTiO₃ photocatalyst as probed by photo-oxidative deposition of PbO₂, indicating that the water oxidation sites are located at the interface between Pt and SrTiO₃. Electron paramagnetic resonance and scanning transmission electron microscope studies suggest that the interfacial oxygen atoms between Pt and SrTiO₃ in Pt/SrTiO₃ after POWS are more readily lost to form oxygen vacancies upon vacuum heat treatment, regardless of Pt loading by photodeposition or impregnation methods, which may serve as additional support for the location of the active sites for water oxidation at the interface. Density functional theory calculations also suggest that the oxygen evolution reaction more readily occurs at the interfacial sites with the lowest overpotential. These experimental and theoretical studies reveal that the more active sites for water oxidation are located at the interface between Pt and SrTiO₃, rather than on the surface of SrTiO₃. Hence, the tailor design and control of the interfacial properties are extremely important for the achievement or improvement of the POWS on cocatalyst loaded semiconductor photocatalyst.

Key words: Photocatalytic overall water splitting, Active site, Oxygen vacancy, Interface, Cocatalyst

Xianwen Zhang, Zheng Li, Taifeng Liu, Mingrun Li, Chaobin Zeng, Hiroaki Matsumoto, Hongxian Han. Water oxidation sites located at the interface of Pt/SrTiO₃ for photocatalytic overall water splitting[J]. Chinese Journal of Catalysis, 2022, 43(8): 2223-2230.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(21)64048-2

https://www.cjcatal.com/EN/Y2022/V43/I8/2223

Figures/Tables 7

Fig. 1. (a) HAADF-STEM and EDS mapping images of P-Pt/STO after photooxidation deposition of PbO2. (b) Diagram of PbO2 photooxidation deposition on the P-Pt/STO surface.

Fig. 2. (a,b) EPR spectra of P-Pt/STO and STO samples before and after vacuum heat treatment. (c) P-Pt/STO samples were further treated with oxygen heat treatment after vacuum heat treatment. Va: vacuum at room temperature for 1 h. Va-400: vacuum heat treatment at 400 °C for 1 h. Va-400-O2: further treated with oxygen heat treatment at 250 °C for 1 h after vacuum heat treatment. All EPR spectra were tested under vacuum at 295 K. (d) TGA curve of P-Pt/STO sample in argon containing 10% oxygen.

Fig. 3. (a) ABF-STEM image of the P-Pt/STO sample after vacuum heat treatment. The red doted circles indicate the oxygen vacancy. (b) The enlarged ABF-STEM image of the dotted line region in Fig. 3(a). The red circles, green circles and yellow circles represent oxygen, strontium and titanium atoms, respectively. (c) The line profiles along the [100] axis corresponding to the dotted line in Fig. 3(b).

Fig. 4. (a) POWS activities of I-Pt/STO. Reaction conditions: photocatalyst, 300 mg; de-ionized H2O, 150 mL; light source, Xenon lamp (300 W). (b) Before and after POWS, EPR spectra of I-Pt/STO samples which were treated with vacuum heat treatment before EPR test. All EPR spectra were tested under vacuum measured at 23 °C.

Fig. 5. In situ ABF images of I-Pt/STO samples after POWS test during vacuum heat treatment process.

Fig. 6. The structural model of the OER intermediates on (100) surfaces. (a) (100); (b) (100)-OH; (c) (100)-O; (d) (100)-OOH. The red, gray, green and white spheres represent for O, Ti, Sr and H atoms, respectively. (e) Free energy diagram of water oxidation on STO (100) surface.

Fig. 7. The structural model of the OER intermediates on (100)-Pt4 surfaces. (a) (100)-Pt4; (b) (100)-Pt4-OH; (c) (100)-Pt4-O; (d) (100)-Pt4-OOH. The red, gray, green, white and blue spheres represents for O, Ti, Sr, H and Pt atoms, respectively. (e) Free energy diagram for water oxidation at the interface between Pt4 and STO (100).

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Water oxidation sites located at the interface of Pt/SrTiO₃ for photocatalytic overall water splitting

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