How does anodization time affect morphological and photocatalytic properties of iron oxide nanostructures?

doi:10.1016/j.jmst.2019.07.046

Abstract

Abstract:

Iron oxide nanostructures are promising materials to be used as photocatalysts in different photoelectrochemical applications. There are different techniques in order to synthesize these nanostructures, but one of the most inexpensive and simple method is electrochemical anodization. This method can lead to different nanostructures by controlling its parameters. Anodization time is one of the most critical parameters since it considerably affects the properties of the obtained nanostructures. In this work, different anodization times (5, 10, 15, 30 and 60 min) were studied. The resulting nanotubes were characterized by field emission scanning electron microscopy, Raman laser confocal microscopy, water splitting measurements, Mott-Schottky analysis and electrochemical impedance spectroscopy, in order to test their viability for being used as photocatalysts in photoelectrochemical applications. Results showed that the best photocurrent density values in water splitting tests (0.263 mA m^-2) were achieved for the sample anodized for 10 min under hydrodynamic conditions.

Key words: Iron oxide, Metallic nanostructures, Photoelectrochemistry, Anodization, Time

Lucas-Granados Bianca, Sánchez-Tovar Rita, M. Fernández-Domene Ramón, María Estívalis-Martínez José, García-Antón José. How does anodization time affect morphological and photocatalytic properties of iron oxide nanostructures?[J]. J. Mater. Sci. Technol., 2020, 38: 159-169.

Figures/Tables 14

Fig. 1. Current density versus time registers of the samples anodized in EG +3 vol.% H2O + 0.1 M NH4F during different times: (a) 5 min; (b) 10 min; (c) 15 min; (d) 30 min; (e) 60 min.

Fig. 2. FE-SEM images of the samples anodized for 5 min under static (a, b) and hydrodynamic (c, d) conditions.

Fig. 3. FE-SEM images of the samples anodized for 10 min under static (a, b) and hydrodynamic (c, d) conditions.

Fig. 4. FE-SEM images of the samples anodized for 15 min under static (a, b) and hydrodynamic (c, d) conditions.

Fig. 5. FE-SEM images of the samples anodized for 30 min under static (a, b) and hydrodynamic (c, d) conditions.

Fig. 6. FE-SEM images of the samples anodized for 60 min under static (a, b) and hydrodynamic (c, d) conditions.

Fig. 7. FE-SEM cross section images of the samples anodized under static (a, c, e, g, i) and hydrodynamic (b, d, f, h, j) conditions for 5 min (a, b), 10 min (c, d), 15 min (e, f), 30 min (g, h) and 60 min (i, j).

Table 1 Length measurements of the different iron oxide nanostructures synthesized at different anodization times under both static and hydrodynamic conditions.

Rotation speed/rpm	Anodization time/min	Length/nm
0	5	700
1000	5	500
0	10	950
1000	10	900
0	15	800
1000	15	900
0	30	900
1000	30	800
0	60	500
1000	60	900

Fig. 8. Raman spectra of the nanostructure synthesized for 5 min in EG +3 vol%. H2O + 0.1 M NH4F under static conditions.

Fig. 9. Photocurrent density versus applied potential measurements for the samples anodized at different times under static (a) and hydrodynamic conditions (b). Solar simulated light AM 1.5 (100 mW cm-1) was used for light conditions and 1 M KOH as electrolyte.

Table 2 Current density values measured at 0.5 V (vs. Ag/AgCl) for the different synthesized iron oxide nanostructures.

Rotation speed / rpm	Anodization time/min	i/mA cm^-2
0	5	0.125
	10	0.150
	15	0.150
	30	0.238
	60	0.15
1000	5	0.140
	10	0.263
	15	0.193
	30	0.140
	60	0.140

Fig. 10. Mott-Schottky plots under dark conditions of the samples anodized at different anodization times under static (a) and hydrodynamic (b) conditions.

Fig. 11. Mott-Schottky plots under light conditions of the samples anodized at different anodization times under static (a) and hydrodynamic (b) conditions.

Table 3 ND and EFB values of the different synthesized iron oxide nanostructures.

Anodization time/min	Electrode rotation speed / rpm	Conditions	N_D/cm^-3	E_FB/V vs. Ag/AgCl
5	0	Dark	6.45 × 10²⁰	-0.62
	0	Light	7.33 × 10²⁰	-0.62
	1000	Dark	1.23 × 10²⁰	-0.59
	1000	Light	2.05 × 10²⁰	-0.63
10	0	Dark	3.93 × 10¹⁹	-0.66
	0	Light	7.30 × 10¹⁹	-0.71
	1000	Dark	4.24 × 10¹⁹	-0.70
	1000	Light	6.28 × 10¹⁹	-0.75
15	0	Dark	5.06 × 10¹⁹	-0.72
	0	Light	1.52 × 10²⁰	-0.80
	1000	Dark	1.02 × 10¹⁹	-0.75
	1000	Light	2.21 × 10¹⁹	-0.77
30	0	Dark	4.00 × 10²⁰	-0.72
	0	Light	5.34 × 10²⁰	-0.80
	1000	Dark	3.25 × 10²⁰	-0.81
	1000	Light	3.69 × 10²⁰	-0.82
60	0	Dark	6.35 × 10²⁰	-0.69
	0	Light	1.14 × 10²¹	-0.73
	1000	Dark	2.48 × 10²⁰	-0.72
	1000	Light	3.20 × 10²⁰	-0.81

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