Photoelectrochemical Degradation of Organic Compounds Coupled with Molecular Hydrogen Generation Using Electrochromic TiO2 Nanotube Arrays

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Division of Environmental Science and Engineering, Pohang University of Science and Technology (POSTECH), Pohang 37673, Korea
School of Chemical and Biological Engineering, Seoul National University, Seoul 151-742, Korea
*Phone: +82-54-279-2283; e-mail: [email protected]
Cite this: Environ. Sci. Technol. 2017, 51, 11, 6590–6598
Publication Date (Web):April 26, 2017
https://doi.org/10.1021/acs.est.7b00774
Copyright © 2017 American Chemical Society
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Abstract

Vertically aligned TiO2 nanotube arrays (TNTs) were prepared by electrochemical anodization, and then cathodically polarized with dark blue coloration for the dual-functional photoelectrochemical water treatment of organic substrates degradation and accompanying H2 generation. The resulting Blue-TNTs (inner diameter: ∼40 nm; length: ∼9 μm) showed negligible shift in X-ray diffraction pattern compared with the intact TNTs, but the X-ray photoelectron spectra indicated a partial reduction of Ti4+ to Ti3+ on the surface. The electrochemical analyses of Blue-TNTs revealed a marked enhancement in donor density and electrical conductivity by orders of magnitude. Degradations of test organic substrates on Blue-TNTs were compared with the intact TNTs in electrochemical (EC), photocatalytic (PC), and photoelectrochemical (PEC) conditions (potential bias: 1.64 VNHE; λ > 320 nm). The degradation of 4-chlorophenol was greatly enhanced on Blue-TNTs particularly in PEC condition, whereas the PC activities of the Blue- and intact TNTs were similar. The potential bias of 1.64 VNHE did not induce any noticeable activity in EC condition. Similar trends were observed for the degradation of humic acid and fulvic acid, where main working oxidants were found to be the surface hydroxyl radical as confirmed by hydroxyl radical probe and scavenger tests. H2 generation coupled with the organic degradation was observed only in PEC condition, where the H2 generation rate with Blue-TNTs was more than doubled from that of intact TNTs. Such superior PEC activity was not observed when a common TiO2 nanoparticle film was used as a photoanode. The enhanced electric conductivity of Blue-TNTs coupled with a proper band bending in PEC configuration seemed to induce a highly synergic enhancement.

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The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.est.7b00774.

  • SEM image of intact TNTs (Figure S1); XRD patterns of TNTs and Blue-TNTs (Figure S2); HPLC analysis of 4-CP degradation intermediates (Figure S3); Fluorescence emission spectra of FA (Figure S4) and HA (Figure S5); Fluorescence emission spectra of 7-HC (Figure S6) and 2-HTA (Figure S7) generated on TNTs and Blue-TNTs; Effects of electrolytes on the PEC degradation of 4-CP (Figure S8); Effects of TBA and EDTA on PEC degradation of 4-CP (Figure S9); Comparison of PEC and EC degradation of 4-CP with different bias potentials (Figure S10); XPS Ti 2p band of Blue-TNTs before and after PEC experiment (Figure S11) (PDF)

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