Facile Synthesis of Novel Redox-Mediator-free Direct Z-Scheme CaIn2S4 Marigold-Flower-like/TiO2 Photocatalysts with Superior Photocatalytic Efficiency

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Department of Environmental Engineering, Kyungpook National University, 80 Daehakro, Bukgu, Daegu 702-701, Republic of Korea
Cite this: ACS Appl. Mater. Interfaces 2015, 7, 31, 17138–17154
Publication Date (Web):July 17, 2015
Copyright © 2015 American Chemical Society
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Novel redox-mediator-free direct Z-scheme CaIn2S4 marigold-flower-like/TiO2 (CIS/TNP) photocatalysts with different CaIn2S4 weight percentages were synthesized using a facile wet-impregnation method. Uniform hierarchical marigold-flower-like CaIn2S4 (CIS) microspheres were synthesized using a hydrothermal method. Field-emission scanning electron microscopy and transmission electron microscopy analyses suggested that the formation and aggregation of nanoparticles, followed by the growth of petals or sheets and their subsequent self-assembly, led to the formation of the uniform hierarchical marigold-flower-like CIS structures. The photocatalytic degradation efficiency of the direct Z-scheme CIS/TNP photocatalysts was evaluated through the degradation of the pharmaceutical compounds isoniazid (ISN) and metronidazole (MTZ). The direct Z-scheme CaIn2S4 marigold-flower-like/TiO2 (1%-CIS/TNP) photocatalyst showed enhanced performance in the ISN (71.9%) and MTZ (86.5%) photocatalytic degradations as compared to composites with different CaIn2S4 contents or the individual TiO2 and CaIn2S4. A possible enhancement mechanism based on the Z-scheme formed between the CIS and TNP for the improved photocatalytic efficiency was also proposed. The recombination rate of the photoinduced charge carriers was significantly suppressed for the direct Z-scheme CIS/TNP photocatalyst, which was confirmed by photoluminescence analysis. Radical-trapping studies revealed that photogenerated holes (h+), OH, and O2•– are the primary active species, and suggested that the enhanced photocatalytic efficiency of the 1%-CIS/TNP follows the Z-scheme mechanism for transferring the charge carriers. It was further confirmed by hydroxyl (OH) radical determination via fluorescence techniques revealed that higher concentration of OH radical were formed over 1%-CIS/TNP than over bare CIS and TNP. The separation of the charge carriers was further confirmed using photocurrent and electron spin resonance measurements. Kinetic and chemical oxygen demand analyses were performed to confirm the ISN and MTZ degradation. The results demonstrated that the direct Z-scheme CIS/TNP photocatalyst shows superior decomposition efficiency for the degradation of these pharmaceuticals under the given reaction conditions.

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Chemicals and materials, photocatalysts characterization details, spectral distribution of the light source, FE-SEM and TEM analyses of CIS, FE-SEM-EDX and elemental mapping analyses of 10%-CIS/TNP, XPS survey and high-resolution spectra of 1 and 10%-CIS/TNP, surface area and pore size distribution analysis results, calculation of VB and CB positions of CIS and TNP, and recyclability test of 1%-CIS/TNP photocatalyst. The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acsami.5b03935.

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