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Article history: The influence of the photovoltaic effect on metal corrosion is investigated in this paper by preparing TiO2,
Received 22 June 2019 g-Fe2O3, and NiO nanoparticles connected with metals. The photo-induced protection and corrosion
Received in revised form performance is analyzed by the photoelectrochemical performance and corrosion morphology. The n-
7 October 2019
type semiconductor TiO2 and p-type semiconductor NiO provide protection for coupled 304 stainless
Accepted 19 October 2019
Available online 23 October 2019
steel and Q235 carbon steel. While g-Fe2O3 induces corrosion acceleration of Q235 carbon steel and
corrosion retardation of 304 stainless steel, respectively. Photo-induced protection and corrosion is
determined by the flat band potential of the semiconductor and the corrosion potential of the coupled
Keywords:
Semiconductor-metal heterojunction
metal, which induces inner electric field that driving charge transfer. Additionally, the redox potential of
Photo-induced protection electrolyte influences the photo-induced corrosion performance. This paper provides a comprehensive
Photo-induced corrosion understanding of the photo-induced corrosion and protection.
Flat band potential © 2019 Elsevier B.V. All rights reserved.
Corrosion potential
https://doi.org/10.1016/j.jallcom.2019.152746
0925-8388/© 2019 Elsevier B.V. All rights reserved.
2 Y. Xu et al. / Journal of Alloys and Compounds 817 (2020) 152746
establishing the relationship between the flat band potential of microscope (Axio Lab A1, ZEISS, Germany).
semiconductor, corrosion potential of metal and redox potential of Photoelectrochemical performance was measured with a three-
electrolyte is vital to improve protection effect and minimize het- electrode system on an electrochemical workstation (CHI660E,
erojunction corrosion under irradiation. Shanghai Chenhua Instrument Co. Ltd, Shanghai, China). The
The semiconductor TiO2 has been reported to possess photo- reference electrode and counter electrode were saturated calomel
induced protection [11,12,16,18,20,34], while g-Fe2O3 has been electrode (SCE) and platinum electrode, respectively. A schematic
recognized for corrosion performance [23,24]. Both are prepared illustration of the experimental setup for the electrochemical test is
for use in this study, along with the p-type semiconductor NiO. The shown in Fig. 1. Removal of platinum electrode was only used in the
semiconductors were connected to 304 SS and Q235 CS to construct OCP test [39,40]. The photoelectrochemical cell with the photo-
different semiconductor-metal heterojunctions. Semiconductor electrode and the corrosion cell with the metal electrode were
electrodes were prepared and connected to the metal by copper connected by sodium ion semipermeable membrane. Then, 0.2 M
lines rather than coating on the metal surface to avoid the barrier NaOH containing 0.1 M Na2S redox solution and 3.5 wt % NaCl so-
effect of corrosion products in the corrosion process. This process lution were used in the photoelectrochemical cell, while 3.5 wt %
also aids in the distinguishing of heterojunction corrosion and self- NaCl solution were always used in the corrosion cell. The S2 was
corrosion by the open circuit potential (OCP) changes. The protec- used as a photogenerated holes scavenger to improve photo
tion or corrosion effect of the semiconductors is investigated quantum efficiency of the photoelectrode, and NaOH could inhibit
through the photoelectrochemical performance and electron the hydrolysis of S2. A 3.5 wt % NaCl solution was used to simulate
structure analysis of the semiconductor-metal heterojunctions. The a seawater environment. The photoelectrode and the metal elec-
relationship between the heterojunction structure and charge trode were connected outside by copper wire, which was used as
transfer direction is also investigated. the work electrode. A 300 W xenon lamp with 350 nme780 nm
wavelength with power energy density ¼ 1 W/cm2 (CEL-HXF300,
2. Material and methods Beijing Zhongjiaojinyuan Technology Co. Ltd., China) was used as a
light source. The potentiodynamic polarization curves were tested
2.1. Sample preparation in a potential range of 1e1 VSCE with 0.01 V/s scan rate. Mott-
Schottky plots were then carried out in 0.5 M Na2SO4 solution at
Synthesis of TiO2 nanoparticles were carried out according to the frequency of 5 Hz by 5 mV alternating current amplitude.
the authors’ previous paper [35]. Butyl titanate (C16H36O4Ti), the
precursor of TiO2, was mixed with 45 ml ethanol and 4 ml acetic 3. Results and discussion
acid with vigorous stirring for 10 min. It was then added to a
mixture solution of 35 ml ethanol, 15 ml deionized water, and 4 ml 3.1. Photoelectrochemical performance and corrosion morphology
acetic acid. After a hydrothermal process at 180 C for 12 h, the
resulting precipitate was centrifuged with deionized water and The anatase TiO2, maghemite-Q g-Fe2O3, and NiO nanoparticles
dried at 60 C for 12 h. are synthesized, as confirmed by the x-ray diffraction (XRD) pat-
The g-Fe2O3 nanoparticles were synthesized according to the terns and transmission electron microscopy (TEM) morphology
coprecipitation reaction scheme [36]. Next, FeCl36H2O (0.02 mol) analysis in Fig. S1. The OCP curves of the prepared samples coupled
and FeSO47H2O (0.01 mol) were dissolved in 20 ml and 10 ml with 304 SS in 0.1 M Na2S and 0.2 M NaOH mixture solution were
deionized water, respectively. The two solutions were mixed and then tested, as illustrated in Fig. 2. Photogenerated electrons
added to 200 ml of 0.6 M ammonium hydroxide solution, followed transfer from semiconductors to metal induces the potential
by the addition of NH3H2O (99%) to adjust the pH value to 10e11. decrease rapidly when xenon lamp irradiation is switched on
The precipitate was centrifuged with deionized water and dried at [41,42]. Meanwhile, the photogenerated holes capture electrons
60 C for 12 h to obtain g-Fe2O3 nanoparticles. from the electrolyte. The OCP reaches a final steady-state value
The NiO nanoparticles were synthesized using a sol-gel scheme (photo-induced voltage) until the electron migration and the
[37]. Nickel acetate (C4H6O4Ni4H2O) was dissolved into 40 ml electrolyte reaction approach equilibrium. The average voltage
ethanol with vigorous stirring at 60 C for 1 h. The obtained green difference between light and dark state in three lights on-off cycle
gel was dried at 150 C for 1 h, then adjusted to room temperature is represented as photo-induced voltage drop, which is used to
for 1 day, followed by calcinations in a muffle furnace at 500 C for qualitatively characterize photo-induced protection or corrosion.
2 h (the heating rate is 2 C/min). The photo-induced voltage drop is an important parameter to
evaluate the photo-induced protection performance [27,33]. The
2.2. Preparation of electrodes TiO2 and g-Fe2O3 electrodes exhibit an average voltage drop
of 100 mV and 38 mV, respectively, while NiO exhibits an
The as-prepared powder (0.01 g) was ultrasonically dispersed in average voltage drop of 17 mV as a hole-type semiconductor. The
ethanol (1 ml) for 5 min. Photoelectrodes were then prepared by photo-induced voltage drop increase means more electron transfer
evenly coating the obtained dispersion liquid on the conductive from the semiconductor to the connected metal, resulting in better
side of the indium-tin oxide (ITO) glass and blast drying [38]. The photo-induced protection.
effective area was 3 3 cm2. The metal electrodes were prepared The Q235 CS is coupled with the prepared semiconductors to
by inlaying polished 304 SS or Q235 CS (<1200#) in epoxy resin construct a different inner electric field as it possesses a different
with the working area of 10 10 mm2 exposed. corrosion potential compared with 304 SS [12,16]. The OCP curves
of the galvanic couple of Q235 CS and photoelectrodes in 0.1 M Na2S
2.3. Characterization and 0.2 M NaOH mixture solution are illustrated in Fig. 3. The
overall decline in the three curves is due to the self-corrosion of
The UVevis diffuse reflection spectra (UV-DRS, model No.uv- Q235 CS [43]. Both TiO2 and NiO provide photo-induced protection
3101pc, Japan) of the prepared powders were carried out with for Q235 CS as the photo-induced voltage drop can be detected
BaSO4 as the internal reference standard. The surface morphology when the light is on. The average voltage drop for TiO2 is 42 mV
of metals was recorded using a three-dimensional surface and the average voltage drop for NiO is 3 mV, as seen in Fig. 3(a)
morphology (Zeta-20, America) apparatus and metallographic and (b). For g-Fe2O3, the potential continues to decline due to the
Y. Xu et al. / Journal of Alloys and Compounds 817 (2020) 152746 3
Fig. 3. Open circuit potential of galvanic couple of Q235 carbon steel with TiO2 (curve a), g-Fe2O3 (curve b) and NiO (curve c) in 0.1 M Na2S and 0.2 M NaOH mixture solution with
the xenon lamp irradiation switched on and off intermittently. The 3D surface morphology of Q235 CS (d) coupling with g-Fe2O3 in 0.1 M Na2S and 0.2 M NaOH mixture solution
with irradiation for 40 min.
Fig. 4. Open circuit potential of galvanic couple of Q235 carbon steel with g-Fe2O3 in 3.5 wt % NaCl solution with the xenon lamp irradiation on and off intermittently (a). The 3D
surface morphology of Q235 CS coupling with g-Fe2O3 in 3.5 wt % NaCl solution without (b) and with (c) irradiation for 40 min.
corrosion current density (Icorr) are listed in Table 1 and Table 2. The current of the metal. Photocurrent can’t be distinguished from
corrosion potential of bare 304 SS in dark and under illumination in corrosion current in the potentiodynamic polarization curves. TiO2
3.5 wt % NaCl solution is 0.42 and 0.55 VSCE, respectively. The andg-Fe2O3 provide photo-induced protection for the coupled 304
corrosion potentials of TiO2, g-Fe2O3, and NiO coupling 304 SS SS as illustrated by the potential analysis and surface morphology.
electrode are 0.75, 0.69, and 0.75 VSCE, respectively. UV illu- The increased Icorr was caused by the photocurrent of the n-type
mination will cause the corrosion acceleration of the 304 SS while semiconductors. The p-type NiO-304 SS coupling electrode exhibits
the Ecorr value shifts negatively and the Icorr value increase under the minimum Icorr as the weak photovoltaic effect of NiO. In addi-
illumination [47]. The Ecorr negative shift of the TiO2, g-Fe2O3, and tion, the corrosion potential of bare Q235 CS in dark and under
NiO connected electrodes (Fig. 6(a)) is caused by the photo- illumination in 3.5 wt % NaCl solution is 0.58 and 0.64 VSCE,
generated electrons transfer from the semiconductors to the respectively. The corrosion potential of g-Fe2O3 and Q235 CS
metals. This leading to photo-induced protection of 304 SS as the coupling electrode is 0.48 VSCE with irradiation. The corrosion
surface morphology has confirmed. The Icorr of the coupling elec- pits morphology and potentiodynamic polarization curves suggest
trodes includes photocurrent of the semiconductor and corrosion that the corrosion process of Q235 CS is accelerated by g-Fe2O3
Y. Xu et al. / Journal of Alloys and Compounds 817 (2020) 152746 5
Fig. 5. The 3D surface morphology of bare Q235 CS in 3.5 wt % NaCl solution and with direct irradiation for 40 min.
Fig. 6. The potentiodynamic polarization curves and surface morphology after polarization test of bare 304 SS, Q235 CS in dark and under illumination, 304 SS-semiconductor
(0.1 M Na2S and 0.1 M NaOH mixture solution in photoelectrochemical cell) and Q235 CS-semiconductor (3.5 wt % NaCl solution in photoelectrochemical cell) coupling electrode.
Table 2
The corrosion potential and corrosion current density of bare Q235 CS and Q235 CS- 1 2 kT
¼ E Ef for n type semiconductor
semiconductor coupling electrodes. C 2 eεr ε0 NA2 e
Samples Ecorr (VSCE) Icorr (uA.cm2) (1)
bare Q235 CS dark 0.58 16.8
bare Q235 CS illumination 0.64 64.1
1 2 kT
g-Fe2O3-Q 235 CS illumination 0.48 84.4 ¼ E E f þ for p type semiconductor
C2 eεr ε0 NA2 e
(2)
under irradiation (Fig. 6(b)). UV illumination would also cause the
corrosion acceleration of the metal. But the acceleration is less than where the C is the space-charge capacitance, the e, εr, ε0, N and A is
the photo-induced corrosion. the electronic charge, relative dielectric constant of the semi-
conductor, permittivity of vacuum, major carrier concentration and
effective surface area of the semiconductors, respectively. E is the
6 Y. Xu et al. / Journal of Alloys and Compounds 817 (2020) 152746
applied potential, Ef is the flat band potential, k is Boltzman con- TiO2 and NiO is higher than the corrosion potential of 304 SS and
stant, T is the temperature in K. The kT/e is generally small and can Q235 CS, while g-Fe2O3 is higher than that of 304 SS. For n-type
be neglected [51]. semiconductor TiO2 and g-Fe2O3, when the semiconductor and 304
The M S plots of TiO2, g-Fe2O3, and NiO are provided in Fig. 7. SS are connected electrically to construct a new electron system,
Positive slopes are observed in the TiO2 and g-Fe2O3 plots, electrons in the conduction band spontaneously flow to the metal
demonstrating that the prepared TiO2 and g-Fe2O3 are n-type from the semiconductor before lights on. This occurs until the
semiconductors. For p-type semiconductor NiO, only a negative system reaches a balanced Fermi level. Thus the metal surface ac-
slope is observed. The flat band potential can be estimated by the quires more electrons due to the negative charge accumulation. In
linear parts of the curves extrapolating the plots to 1/C2 ¼ 0, which addition, the electron migration away causes an excess positive
is 0.89, 0.44, and 1.31 VSCE (equal to 3.85, 4.30, 6.07 eV vs charge in the semiconductor, leading to the formation of an inner
vacuum, respectively) for TiO2, g-Fe2O3, and NiO, respectively. For electric field in the semiconductor-metal heterojunction. The
n-type semiconductor, the flat band potential is approximately semiconductor surface band energy bends upward [12]. The
equal to the conduction band bottom (ECB) and for p-type semi- electron-depleted layer forms at the semiconductor side while the
conductor equal to the valence band top (EVB) [52]. Schottky barrier (Øns) forms in the heterojunction interface [31].
The band gap of semiconductors can be estimated using the Consequently, one-way electron migration from semiconductor to
equation: ahn ¼ ðhn EgÞn=2 , where a is the absorption coefficient, metal will occur in the semiconductor-metal heterojunction. When
h is the Planck constant,n is the frequency, Eg is the band gap, and n light is on, Schottky barrier and the potential difference of the inner
is the parameter dependent on the transition type of electrons in electric field increase along with the potential of the semiconductor
the semiconductor. The value of parameter n is 1 for the direct decreases [41]. The photogenerated electrons in the conduction
transition semiconductor, and 4 for the indirect transition semi- band migrate through the electron-depleted layer to the coupled
conductor. Fig. 8 shows the diffuse reflection spectra of the as- metal, resulting in photo-induced protection. The electron potential
synthesized samples (insets) and the corresponding plots of in TiO2 and g-Fe2O3, which is equal to ECB, is 3.85 and 4.30 eV vs
ðahnÞ2=n versus hn. The band gap of TiO2 is estimated to be 3.18 eV vacuum, respectively, as shown in Fig. 9. Thus the Schottky barrier
by extrapolating the straight portion of ðahnÞ1=2 versus hn plots to and the inner electric field in TiO2-304 SS junction is higher than
the point a ¼ 0 (Fig. 8 (a)) as an indirect band gap semiconductor that in g-Fe2O3-304 SS junction. This indicates more electron
[53]. The band gap of g-Fe2O3 and NiO [54,55] is estimated to be transfer and better photo-induced protection, which is consistent
1.58 eV and 3.20 eV by extrapolating the straight portion of ðahnÞ2 with the results of photoelectrochemical performance and corro-
versus hn as direct band gap semiconductors (Fig. 8(b) and (c)). sion morphology.
Fig. 9 schematically illustrates the proposed mechanism of the For p-type semiconductor NiO, electrons will flow from the
photo-induced protection and corrosion. The ECB of TiO2, g-Fe2O3, coupled metal to NiO due to the difference of electrochemical po-
and NiO is 3.85, 4.30, 2.87 eV vs vacuum, respectively, which tential, thus leading to a downward band toward the body [56]. The
are estimated by the M S in Fig. 7 and Eg in Fig. 8. The Ecorr of bare hole-depleted layer and a barrier (Øps) for holes form at the semi-
304 SS and Q235 CS in dark is 4.32 and 4.16 eV vs vacuum, conductor side. When the light is turned on, the potential of the
respectively, which is obtained by the potentiodynamic polariza- NiO electrode decreases. Electrons flow from metal to NiO will
tion curves. It can be observed that the conduction band bottom of decline as the potential difference of the inner electric field
Fig. 7. The Mott-Schottky plots of the prepared TiO2, g-Fe2O3 and NiO photoelectrodes in 0.5 M Na2SO4 solution.
Y. Xu et al. / Journal of Alloys and Compounds 817 (2020) 152746 7
Fig. 8. UVevis diffuse reflection spectra and the corresponding plots of (ahn)2/n versus hn of TiO2 (a), g-Fe2O3 (b), and NiO (c).
declines. The OCP curves exhibits change to negative direction the Q235 CS dissolution, leading to the corrosion acceleration of
under illumination, resulting in photo-induced protection. How- Q235 CS. Meanwhile, the photogenerated hole will also capture
ever, the average voltage drop of NiO electrodes is insufficient electrons from the electrolyte. In comparison to O2/H2O, S/S2
compared with that of TiO2 and g-Fe2O3 electrodes as illustrated in possesses an increased negative redox potential, leading to more
Figs. 2 and 3. Here, p-type semiconductor NiO is not ideal candi- photogenerated electrons accumulation on the surface of g-Fe2O3,
dates for photo-induced protection due to its major carrier and thus reducing the potential difference of the inner electric field
positive flat band potential. between g-Fe2O3 and Q235 CS that decreases the photo-induced
Furthermore, g-Fe2O3 is found to induce corrosion acceleration corrosion effectively.
of Q235 CS under illumination. The conduction band bottom of g-
Fe2O3 is lower than the corrosion potential of Q235 CS. Likewise, 4. Conclusions
spontaneous electron migration forms the inner electric field. The
direction of the inner electric field is from g-Fe2O3 to Q235 CS, Charge transfer happening in the semiconductor-metal hetero-
leading to a downward band bending towards the body. The junction was investigated by preparing TiO2, g-Fe2O3, and NiO
reverse-barrier layer forms at the semiconductor side. When the nanoparticles connected with metals in this work. Inner electric
light is on, photogenerated electron will not transfer to the coupled field formed in the heterojunction interface determines the elec-
Q235 CS due to the existence of barrier (ØA). Inversely, photo- trons or holes migrate. Photo-induced protection for 304 SS and
generated holes generated in g-Fe2O3 will capture electrons from Q235 CS was provided by TiO2, as it conduction band bottom is
8 Y. Xu et al. / Journal of Alloys and Compounds 817 (2020) 152746
higher than the corrosion potential of the coupled metal. P-type characteristics of In2S3 nano-flower films on TiO2 nanorods arrays, Appl. Surf.
Sci. 369 (2016) 108e114.
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