Structural engineering of 3D hierarchical Cd0.8Zn0.2S for selective photocatalytic CO2 reduction

doi:10.1016/S1872-2067(20)63623-3

Abstract

Abstract:

The solar-driven catalytic conversion of CO₂ to useful chemical fuels is regarded as an environmentally friendly approach to reduce the consumption of fossil fuels and mitigate the greenhouse effect. However, it is highly intriguing and challenging to promote the selectivity and efficiency of visible-light-responsive photocatalysts that favor the adsorption of CO₂ in photoreduction processes. In this work, three-dimensional hierarchical Cd_0.8Zn_0.2S flowers (C8Z2S-F) with ultrathin petals were successfully synthesized through an in-situ self-assembly growth process using sodium citrate as a morphology director. The flower-like Cd_0.8Zn_0.2S solid solution exhibited remarkable photocatalytic performance in the reduction of CO₂, generating CO up to 41.4 μmol g^-1 under visible-light illumination for 3 h; this was nearly three times greater than that of Cd_0.8Zn_0.2S nanoparticles (C8Z2S-NP) (14.7 μmol g^-1). Particularly, a comparably high selectivity of 89.9% for the conversion of CO₂ to CO, with a turnover number of 39.6, was obtained from the solar-driven C8Z2S-F system in the absence of any co-catalyst or sacrificial agent. Terahertz time-domain spectroscopy indicated that the introduction of flower structures enhanced the light-harvesting capacity of C8Z2S-F. The in situ diffuse reflectance infrared Fourier transform spectroscopy unveiled the existence of surface-adsorbed species and the conversion of photoreduction intermediates during the photocatalytic process. Empirical characterizations and predictions of the photocatalytic mechanism demonstrated that the flower-like Cd_0.8Zn_0.2S solid solution possessed desirable CO₂ adsorption properties and an enhanced charge-transfer capability, thus providing a highly effective photocatalytic reduction of CO₂.

Key words: Cd_0.8Zn_0.2S flowers, Self-assembly growth, Photocatalytic CO₂ reduction, High selectivity, Visible-light irradiation

Lei Cheng, Dainan Zhang, Yulong Liao, Jiajie Fan, Quanjun Xiang. Structural engineering of 3D hierarchical Cd_0.8Zn_0.2S for selective photocatalytic CO₂ reduction[J]. Chinese Journal of Catalysis, 2021, 42(1): 131-140.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(20)63623-3

https://www.cjcatal.com/EN/Y2021/V42/I1/131

Figures/Tables 8

Fig. 1. Morphology and phase structures of the photocatalyst. (a) Schematic of C8Z2S-F synthesis; (b) HAADF-STEM image; (c) TEM image; (d) XRD pattern; (e) SEM image; (f, g) AFM images of C8Z2S-F. The obtained C8Z2S-F was synthesized through a simple oil-bath treatment of CdCl2 and ZnCl2 (the molar ratio of Cd/Zn was 4:1) in thiourea solution with sodium citrate and NH3·H2O as structure directors at 60 °C for 3 h.

Fig. 2. Compositional characterizations and photocatalytic CO2 reduction performance of as-synthesized photocatalysts. (a) XPS spectra; (b) High resolution XPS spectra; (c) N2 adsorption-desorption isotherms (inset indicates the pore size distribution); (d) UV-vis DRS spectra (inset shows the Kubelka-Munk function vs. photon energy curves); (e) Mott-Schottky plots; (f) Schematic of the electronic band structures of the as-obtained C8Z2S-F sample; (g) Photocatalytic products of CO2 reduction detected by original chromatograms over C8Z2S-F and C8Z2S-NP samples under visible-light irradiation for 3 h; Photocatalytic activity of CO (h) and CH4 evolution (i) over C8Z2S-F and C8Z2S-NP samples under visible light irradiation. Reaction conditions: photocatalyst (0.03 g), deionized water (500 μL), Xe lamp (300 W).

Fig. 3. Optical performance of as-synthesized photocatalysts. THz-TDS transmittance (a) and THz-TDS reflectivity (b) of C8Z2S-F and C8Z2S-NP samples.

Fig. 4. Physicochemical properties and mechanism study of as-synthesized photocatalysts. CO2-TPD profiles (a) and EIS spectras (b) (inset shows the TPR curves) of C8Z2S-F and C8Z2S-NP samples; (c) Schematic of the photocatalytic reduction of CO2 by using C8Z2S-F sample as photocatalyst.

Fig. 5. The in situ DRIFTS spectra of CO2 adsorption over as-synthesized C8Z2S-F photocatalysts. Surface photocatalytic intermediates after introduction of CO2 + H2O interaction under dark (0-60 min) and 365 nm light irradiation (60-120 min) in different wavenumber ranges of 1000-1400 cm-1 (a) and 1400-2100 cm-1 (b); (c) schematic of the possible photocatalytic process during the conversion of CO2 to CO and CH4 under visible-light irradiation.

Fig. 6. Morphological characterizations of the photocatalysts. (a1-d1) SEM images; (a2-d2) HAADF-STEM images; (a3-d3) schematic of the structures of C2Z8S, C5Z5S, C8Z2S-F, and C8Z2S-NP samples.

Fig. 7. Comparison of electrochemical characterizations and photocatalytic CO2 reduction performance over a series of photocatalysts. N2 adsorption-desorption isotherms (a) (inset indicates the pore size distribution); UV-vis DRS spectra (b) (inset shows the Kubelka-Munk function vs. photon energy curves), Mott-Schottky plots (c), and EIS spectra (d) (inset presents the TPR curves) of C8Z2S-F, C5Z5S, and C2Z8S samples; Photocatalytic activity of CO (e) and CH4 evolution (f) over C8Z2S-F, C5Z5S and C2Z8S samples under visible-light irradiation. Reaction conditions: photocatalyst (0.03 g), deionized water (500 μL), Xe lamp (300 W).

Table 1 Evaluation of selective CO2 photoconversion.a

Sample	Production rate^b (μmol g^-1 h^-1)		TON ^c	Selectivity for CH₄^d (%)
Sample	CO	CH₄	TON ^c	Selectivity for CH₄^d (%)
C8Z2S-F	17.8	0.5	39.6	89.9
C5Z5S	11.0	0.3	24.4	90.2
C2Z8S	9.5	0.3	21.4	88.8
C8Z2S-NP	4.9	0.4	13	75.4

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Structural engineering of 3D hierarchical Cd_0.8Zn_0.2S for selective photocatalytic CO₂ reduction

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