Enhanced the Performance of Photoelectrochemical Oxidation of Water over BiVO4 Film Electrodes by Electrochemical Reduction Pretreatment†

doi:10.7503/cjcu20130537

Abstract

Abstract:

BiVO₄ thin film electrodes were pretreated by electrochemical reduction(ER) in acid aqueous solutions(pH=2), and its impact on the performance of photoelectrochemical oxidation of water was tested. The results show that this treatment enhances the photoelectrochemical oxidation of water over the BiVO₄ thin film electrodes and the treated electrodes have a good photoelectrochemical stability. The untreated and ER treated electrode films were characterized by scanning electron microscopy, X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, UV-Vis diffuse reflectance spectroscopy, photoluminescence, electrochemical impedance spectroscopy, Mott-Schottky measurements, etc. From a physical chemistry perspective, the ER pretreatment resulted an increase of the roughness of the electrode with increasing in surface area by a factor of 1.4; no detectable change in crystalline but a slightly red-shift in the V—O symmetric stretching; a decrease in binding energy for the surface Bi, V and O; partly reduction of Bi³⁺ with an increase in the atom ratio of Bi/V on the surface. From the view of photoelectrochemistry, due to ER treatment, the flatband potential for the electrode was negatively shifted, the charge-transfer rate of photocarriers at the electrode/solution interface was accelerated while the surface recombination rate was decreased. These changes and the increased surface area are the main reasons for the enhanced photoelectrochemical performance.

Key words: BiVO4, Electrochemical reduction, Photoelectrochemical oxidation of water, Pretreatment

CLC Number:

O643

TrendMD:

LI Haili, ZHU Hongqiao, CAO Fahe, LENG Wenhua. Enhanced the Performance of Photoelectrochemical Oxidation of Water over BiVO₄ Film Electrodes by Electrochemical Reduction Pretreatment^†[J]. Chem. J. Chinese Universities, 2014, 35(2): 377.

Figures/Tables 10

Fig.1 Typical SEM images of BiVO4 electrodes without(A) and with(B) electrochemical reduction(ER)

Fig.2 XRD patterns of BiVO4 electrodes without(a) and with(b) ER

Fig.3 Raman spectra of BiVO4 electrodes without(a) and with(b) ER

Fig.4 XPS spectra of BiVO4 electrodes without(a) and with(b) ER(A) Wide spectra; (B) Bi; (C) V; (D) O element. Dashed and dotted lines in (B)—(D) are fitted and background ones, respectively.

Fig.5 EDS of BiVO4 electrodes without and with ER pretreatment

Table 1 XPS and EDS data of BiVO4 thin films without and with ER

Element	E_b/eV		Peak area^a		Area ratio^b	Mass ratio by EDS^c
Element	without ER	with ER			without ER	with ER
B $i 4 f 52$	158.7	157.3	814	918	0.887	0.881
B $i 4 f 72$	164.2	162.6
$V 2 p 12$	516.1	515.2	892	965	0.924	0.9
$V 2 p 32$	523.7	522.8
O₁_s	520.8	529.4	3830	4026	0.951	0.9

Table 1 XPS and EDS data of BiVO4 thin films without and with ER

Element	E_b/eV		Peak area^a		Area ratio^b	Mass ratio by EDS^c
Element	without ER	with ER			without ER	with ER
B $i 4 f 52$	158.7	157.3	814	918	0.887	0.881
B $i 4 f 72$	164.2	162.6
$V 2 p 12$	516.1	515.2	892	965	0.924	0.9
$V 2 p 32$	523.7	522.8
O₁_s	520.8	529.4	3830	4026	0.951	0.9

Fig.6 Photoelectrochemical performance of BiVO4 thin film electrodes without and with ER pretreatment(A) I-V curves of BiVO4 electrodes in the dark(a, b), under visible(c, d) and UV-Vis light(e, f) illumination. a, c, e. without ER(dark); b, d, f. with ER(dark); (B) corresponding I-t curves of BiVO4 electrodes to Fig.6(A). a. without ER(Vis); b. with ER(Vis); c. without ER(UV-Vis); d. with ER(UV-Vis); e. on FTO without ER(Vis); f. on FTO with ER(Vis); (C, D) photocurrent of BiVO4 electrodes versus ER potential(C) and ER time(D); (E) photoelectrochemical stability; (F) effect of immersion treatment in Ag+ containing solutions[11] on the photoelectrochemical stability of the ER treated BiVO4 electrodes. (C)—(F) with visible light illumination.

Fig.7 Typical EIS under white light(A), charge-transfer rate constant(B), Mott-Schottky curves(C) for the BiVO4 film electrodes without and with ER, and series resistance(Rs) measured at 100 kHz by EIS vs. applied potential for the fresh, ER treated(-0.5 V for 2 min) and sintered(550 ℃ for 0.5 h) ITO and FTO glass(D)(B) a, d. Without ER; b, c. with ER.(C) Efb: flatband potential, R2: relevant coefficient.

Fig.8 Typical EIS responses for the BiVO4 electrodes under white light illumination(A) and in the dark(B, C) without and with ER pretreatment(B) Nyquist; (C) bode.

Fig.9 PL spectra of BiVO4 film electrode without(a) and with(b) ER(A) and relationship of Cp-potential in the dark for the BiVO4 thin film electrodes without(B) and with(C) ER pretreatmenta. 1 Hz; b. 5 Hz; c. 10 Hz.

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Enhanced the Performance of Photoelectrochemical Oxidation of Water over BiVO₄ Film Electrodes by Electrochemical Reduction Pretreatment^†

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