Properties of sodium molybdate-based compound corrosion inhibitor for hot-dip galvanized steel in marine environment

Zhenkai Xu; Lian Chen; Jingliang Han; Chengfei Zhu

doi:10.1515/corrrev-2022-0043

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Properties of sodium molybdate-based compound corrosion inhibitor for hot-dip galvanized steel in marine environment

Zhenkai Xu , Lian Chen , Jingliang Han und Chengfei Zhu

Veröffentlicht/Copyright: 23. Januar 2023

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Abstract

Sodium molybdate (Na₂MoO₄) was selected as the corrosion inhibitor, compounded with benzimidazole, in order to prolong the service life of the hot-dip galvanized steel (HDGS) in the marine environment in this article. XRD, SEM/FESEM and EDS were used to characterize the micro-morphology and elemental composition of HDGS. Immersion corrosion test, Tafel polarization and EIS test were carried out to study the effect of compound inhibitor on the corrosion resistance of HDGS in the marine environment. The best proportion of compound inhibitor was added to the self-made waterborne polyurethane coating (WPUC), aiming to evaluate its influence on the coating performance in the marine environment by immersion corrosion test and EIS test. The results showed that Na₂MoO₄, as a passivation type corrosion inhibitor, bounded Zn at the active sites of HDGS coupons and created structural defects. Benzimidazole, as an adsorption type corrosion inhibitor, was attracted by electricity and adsorbed at the structural defects. Under the premise of 1 wt% total content, the optimal ratio of Na₂MoO₄ & benzimidazole was 9:1 and the corrosion inhibition efficiency was 99.62%. The corrosion current density of HDGS in the simulated seawater with compound inhibitor was 5.650 × 10⁻⁸ A/cm², while that of HDGS in the simulated seawater without compound inhibitor was 1.483 × 10⁻⁵ A/cm². The WPUC containing compound inhibitor had a small decrease in corrosion resistance due to defects created by doping at the beginning of immersion, then the compound inhibitor would play an active role in the corrosion process to make more than double the service life of WPUC.

Keywords: hot-dip galvanized steel; marine environment; sodium molybdate compound corrosion inhibitor; waterborne polyurethane

1 Introduction

Hot-dip galvanized steel (HDGS) is widely used in marine facilities, petroleum industry and other fields due to their characteristics of corrosion resistance, low cost, mature technology and abundant reserves (Al-Negheimish et al. 2021; Nakhaie et al. 2020; Qiao et al. 2019). The production process of HDGS can be briefly described as follows: the steel was immersed in a hot-dip plating reactor, and the molten zinc then reacted with the iron matrix to form an alloy layer (Kancharla et al. 2022; Saber 2021). Hence, the surface of HDGS was combined with a dense zinc layer. On one hand, the galvanized layer can effectively separate the iron matrix from the corrosive medium, making it physically protected (Fan et al. 2020; Zhang et al. 2021). On the other hand, the galvanized layer was corroded first because of the lower corrosion potential, so that the iron matrix can be electrochemically protected (Li et al. 2022; Thanyalux et al. 2021). Therefore, HDGS can maintain properties over a long time. There was also electro-galvanized steel (cold galvanized steel) apart from HDGS. The galvanized layer of electro-galvanized steel was thin and simply attached to the substrate, which was easy to fall off. So the corrosion resistance of electro-galvanized steel wasn’t ideal (An 2017). Hence, electro-galvanized steel had been eliminated and most of the galvanized steel currently used was HDGS. However, several elements, such as Cl and S, can destabilize the HDGS, resulting in the acceleration of corrosion, which limits the application and development of HDGS (Delaunois et al. 2014; Karthick et al. 2020; Roventi et al. 2014). Therefore, further protective technologies are required. Compared with other methods, the corrosion inhibitor is more applicable because it has the advantages of simple operation, less dosage and high efficiency (Auepattana-Aumrung et al. 2022; He et al. 2021; Mobin et al. 2022).

Some progress have been made in the research on corrosion inhibitors for HDGS. Kartsonakis et al.(2016) investigated the principle and the effect of several inhibitions on the corrosion behavior of HDGS in NaCl solution. Gaber et al.(2021) studied the effect of 2-cyano-N-(4-morpholinebenzylbutyl) acetylhydrazide on the corrosion behavior of HDGS in 1M sulfuric acid. Results showed that a smooth and dense adsorption film formed on the surface, and the inhibitor followed the Langmuir adsorption isotherm in an acidic environment. Matis et al.(2021) explored the effect of humic acids on the corrosion behavior of HDGS in high organic matter soils. Results showed that humic acid can combine with the Zn to form a secondary passivation layer, which had the corrosion inhibition effect. But humic acid can also accelerate corrosion in the initial stage.

As a passivation type corrosion inhibitor, Na₂MoO₄ was often used alone or in conjunction with other substances to inhibit the corrosion of carbon steel and stainless steel in various media (Coronel-García et al. 2020). Nguyen et al.(2020) added Na₂MoO₄ to hydrotalcite/ graphene oxide composite and mixed the composite with waterborne epoxy coating. It was found that Na₂MoO₄ can strengthen the corrosion resistance of the coating and improve the protection efficiency to 96%. But the application of Na₂MoO₄ as a corrosion inhibitor for HDGS was not common. Wang et al. (2018) studied the effect of Na₂MoO₄ on the rapid dissolution and hydrogen evolution behavior of HDGS in a new concrete environment. They found that a film containing Mo formed on the corrosion interface to play a barrier effect in a high alkali environment. However, there was no research on corrosion inhibitors for HDGS in the marine environment.

In order to select the corrosion inhibitors for HDGS in the marine environment, the corrosion inhibition mechanism of Na₂MoO₄ compounded with benzimidazole was evaluated in the article. The optimal compound combination was added into the self-made waterborne polyurethane coating (WPUC) to investigate its effect on the comprehensive performance of the coating.

2 Materials and methods

2.1 Materials

Figure 1 presents the schematic diagram of the HDGS coupons, the layers of zinc and coating. The HDGS (99 wt% molten bath zinc) was brought from Baoshan Iron & Steel Co, and then cut into rectangular test pieces, whose size was 50 mm × 25 mm × 0.2 mm. The thickness of the galvanized layer was 45 ± 5 μm. The WPUC was rolled onto HDGS coupons with a film thickness of 1.3 ± 0.1 μm. The Na₂MoO₄ and benzimidazole were purchased from Shanghai Aladdin Co. The simulated seawater was configured according to the Mocledon formula (Yue et al. 2014). The specific components of the simulated seawater were as follows: sodium chloride 26.726 g/L, magnesium chloride 2.26 g/L, magnesium sulfate 3.248 g/L, calcium chloride 1.153 g/L, sodium bicarbonate 0.198 g/L, potassium chloride 0.721 g/L, sodium bromide 0.058 g/L, boric acid 0.058 g/L, sodium silicate 0.0024 g/L, disodium tetrasilicate 0.0015 g/L, phosphoric acid 0.002 g/L, aluminium chloride 0.013 g/L, ammonia 0.002 g/L, lithium nitrate 0.0013 g/L.

Figure 1:

Schematic diagram of HDGS coupons with and without WPUC.

2.2 Synthesis

The HDGS coupons were immersed in ammonium acetate (NH₃CH₂COOH) solution with the concentration of 10 wt% at 70 °C for 5 min first to remove the oxide and then cleaned in deionized water. 5 wt% medium alkaline degreasing agent was applied to degrease the HDGS coupons’ surface by ultrasonic cleaning for 5 min. After washing with deionized water, the HDGS coupons were soaked in absolute ethanol, then dried with cold air for use. After the preliminary experiment, it was determined that the corrosion inhibitor combination was a binary compound of Na₂MoO₄ and benzimidazole with a total content of 1 wt%. The specific ratio and concentration are shown in Table 1. The immersion test was carried out in 25 °C water bath without ventilation. Each group contained three parallel HDGS coupons to reduce error. Each HDGS coupon was immersed in 500 mL of simulated seawater containing corrosion inhibitor for 144 h.

Table 1:

Concentration of Na₂MoO₄ and benzimidazole in compound corrosion inhibitor.

Group	A	B	C	D	E	F	G	H	I	J
Ratio of Na₂MoO₄ to benzimidazole	0:0	1:0	0:1	2:1	5:1	8:1	9:1	10:1	11:1	20:1
C_Na2MoO4 (g/dm³)	0	10	0	6.667	8.333	8.889	9	9.091	9.167	9.524
C_{benzimidazole} (g/dm³)	0	0	10	3.333	1.667	1.111	1	0.909	0.833	0.476

The selected compound corrosion inhibitor was added to the self-made WPUC at a ratio of 1 wt%. Magnetic stirred at 25 °C for 6 h. The WPUC with and without compound inhibitor were roll-coated on HDGS coupons with an RDS wire rod coater (#3, USA), then dried at 200 °C for 37 s. The immersion time of the coated HDGS coupons was extended to 400 h to obtain a complete corrosion process.

2.3 Characterization

The microstructure and composition changes of HDGS coupons were observed by a scanning electron microscope (SEM, HITACHI S-4800, Japan) equipped with an energy dispersive spectrometer (EDS) and a field emission scanning electron microscope (FESEM, Regulus 8100, Japan). The composition of the corrosion product was determined by an X-ray diffractometer (XRD, Rigaku, Japan). The scanning speed was 10°/min in the 2θ ranges from 10° to 90°.

The effect of corrosion inhibitor on the HDGS coupons and WPUC were evaluated by static immersion test. The corrosion area of WPUC was obtained by comparing with the standard square. The corrosion rate of HDGS after being immersed was calculated by formula (1). The inhibition efficiency was calculated by formula (2).

(1)V±=m0−m1S×t

(2)η=V0−V1V0

where V± was the corrosion rate, g/(m²·h); m₀ was the HDGS coupons’ mass before corrosion, g; m₁ was the HDGS coupons’ mass after corrosion, g; S was the area exposed to the solution, m²; t was corrosion time, h; η was the inhibition efficiency, %; V₀ and V₁ were the corrosion rates in the simulated seawater without and with corrosion inhibitor, g/(m²·h), respectively.

Potentiodynamic polarization curves and AC Impedance spectroscopy (EIS) tests of HDGS coupons with and without WPUC coated were performed in simulated seawater at 25 °C via Solartron 1260 + 1287 electrochemical workstation. The saturated Hg/Hg₂Cl₂ electrode and graphite electrode were used as the reference electrode and counter electrode, respectively. The HDGS coupons were the working electrode. During the potentiodynamic polarization measurements, the potential was swept from −300 mV to +300 mV (vs. open circuit potential) using a scan rate of 1 mV/s. The EIS data were obtained in the frequency range of 10⁵–10⁻³ Hz with an amplitude of 0.05 V.

3 Results and discussion

3.1 Corrosion analysis

3.1.1 Static immersion test

Figure 2 depicts the corrosion rate of HDGS in simulated seawater with different inhibitors. The corrosion rate of HDGS in the simulated seawater with no inhibitor added was as high as 221.6 μm/y. The corrosion rate was reduced to 87.33 μm/y with the addition of Na₂MoO₄, while the inhibition efficiency reached 60.59%. Na₂MoO₄ can passivate the Zn layer to form a passivation film, which reduced the penetration rate of the corrosive medium. However, the passivation film couldn’t resist the damage of chloride ions in the marine environment completely. The addition of benzimidazole can reduce the corrosion rate to 9.757 μm/y and increase the efficiency to 95.60%. The N contained in benzimidazole can adsorb on the surface by combining with cations to hinder the exchange of electrons in the process of corrosion and thus play a protective role. However, benzimidazole was not suitable for mass use due to its hydrophobicity and toxicity. Compared with single inhibitors, the compound inhibitors can greatly slow down the corrosion rate regardless of the proportion, indicating further improvement of the inhibition ability. Group G (the ratio of Na₂MoO₄ to benzimidazole was 9:1) was the best ratio concentration, the lowest corrosion rate was 2.208 μm/y, and the inhibition efficiency was up to 99.62%.

Figure 2:

Corrosion rate of HDGS in simulated seawater with different inhibitors.

3.1.2 Potentiodynamic polarization test

Figure 3 shows the potentiodynamic polarization curves of HDGS coupons in simulated seawater containing different inhibitors at 25 °C. The corrosion parameters obtained from the polarization curves are shown in Table 2. It can be seen from the anodic polarization curve of HDGS in simulated seawater rose sharply, while the curve appeared as a gentle slope in the simulated seawater with the compound inhibitors. This process was related to the passivation of MoO₄²⁻ and the adsorption of benzimidazole. Active sites of HDGS were covered, which increased the difficulty of charge exchange and led to a slow increase in corrosion current (Kumar et al. 2021). The corrosion resistance of HDGS (Icorr = 5.650 × 10⁻⁸ A/cm²) under the action of compound inhibitor G was the best, which was consistent with the conclusion of static immersion experiment.

Figure 3:

Polarization curves of HDGS coupons of different groups in simulated seawater at 25 °C.

Table 2:

Fitted data of the polarization curves shown in Figure 3.

Group	Ecorr (V vs. SCE)	Icorr (A/cm²)	η (%)	σ _η (%)
A	−1.013	1.483 × 10⁻⁵	–	–
B	−0.930	6.017 × 10⁻⁶	59.43	0.29
C	−0.884	5.980 × 10⁻⁷	95.97	0.44
D	−0.953	2.999 × 10⁻⁷	97.98	0.43
E	−0.954	2.317 × 10⁻⁷	98.44	0.30
F	−0.899	7.534 × 10⁻⁸	99.49	0.23
G	−1.096	5.650 × 10⁻⁸	99.62	0.16
H	−0.953	1.832 × 10⁻⁷	98.76	0.39
I	−0.911	3.491 × 10⁻⁷	97.65	0.24
J	−0.992	3.975 × 10⁻⁷	97.32	0.28

3.1.3 EIS test

Figure 4 was the electrochemical impedance spectroscopy of HDGS in simulated seawater of different groups. The impedance spectrum without corrosion inhibitor showed a single semicircle, while the impedance spectrum with compound inhibitors were compound flattened semicircle arcs. This phenomenon was associated with interfacial reactions during corrosion (Moya 2018). Only corrosion process occurred on HDGS in simulated seawater without corrosion inhibitor. But the interface reaction occurred not only on the surface of HDGS, but also the film interface formed in simulated seawater with corrosion inhibitor.

Figure 4:

EIS curves of HDGS of different groups in simulated seawater at 25 °C.

Figure 5A and B presents the equivalent circuit model of HDGS in simulated seawater and simulated seawater with different compositions inhibitors, respectively. Where Rs was the solution resistance, CPE was the constant phase angle element, Rf was the resistance of HDGS, CPEdl and Rct were the CPE of the double electric layer and the charge transfer resistance, respectively. The values of equivalent circuit parameters are listed in Table 3. The charge transfer resistance value of group G was the largest of 76,071 Ω·cm². It was consistent with the static immersion test and potentiodynamic polarization test as well.

Figure 5:

Equivalent circuit of HDGS for fitting Nyquist plot.

Table 3:

Electrochemical parameters estimated from EIS experiments.

Group	CPE-T (10⁻⁵·Ω⁻¹·cm⁻²·s⁻ⁿ¹)	n ₁	Rf (kΩ·cm²)	CPEdl-T (10⁻⁵·Ω⁻¹·cm⁻²·s⁻ⁿ²)	n ₂	Rct (kΩ·cm²)
A	18.77	0.76	0.32	–	–	–
B	52.10	0.69	0.78	46.25	0.55	0.66
C	2.07	0.70	2.42	1.33	0.90	1.88
D	9.05	0.73	8.72	12.83	0.56	12.55
E	13.25	0.63	9.66	55.70	0.58	14.43
F	9.19	0.66	31.40	8.85	0.63	27.93
G	31.59	0.51	36.07	48.33	0.54	40.00
H	13.38	0.63	8.57	24.37	0.37	19.03
I	14.11	0.65	13.99	6.12	0.75	5.72
J	16.75	0.64	5.05	30.11	0.51	8.94

3.2 Characterization of HDGS after immersion

Figure 6 presents the SEM morphologies of HDGS after immersion in simulate seawater. Table 4 indicates the EDS analysis of HDGS after immersion. Figure 6A and B shows that the corrosion products formed on HDGS in simulated seawater without corrosion inhibitor were thorny spherical, evenly distributed but loose, which was not enough to protect the matrix. The holes and cracks appeared on the surface of HDGS after immersion in simulate seawater with Na₂MoO₄ (Figure 6C and D), which indicated that the passivation film of Na₂MoO₄ couldn’t completely resist the damage of chloride ions. As Figure 6E and F shows, lamellar and acicular benzimidazole was attached to the surface of HDGS after immersion in simulate seawater with benzimidazole. Figure 6G shows the SEM of HDGS after immersion in simulate seawater with the compound inhibitor. Na₂MoO₄ passivated the matrix to form structural defects. The benzimidazole then attached to the defects to delay the corrosion (Golchinvafa et al. 2020). The N was at a peak value of 1.44 wt%. Figure 6H is the FESEM of the junction surface between the composite inhibitor film and the substrate in Group G. The surface was observed after washing off the film attached to the surface with deionized water. The well-defined spherical molybdate passivators were bonded to each other, as well as the benzimidazole. Benzimidazole was thought to influence the electron donating process of molybdate passivation during the adsorption process (Cheng et al. 2022; Pessu et al. 2021).

Figure 6:

SEM morphologies of HDGS after immersion in simulated seawater in different groups (groups A, B, C and G).

Table 4:

EDS analysis of HDGS after immersion.

Group	A	B	C	D	E	F	G	H	I	J
Mo (wt%)	0	18.92	0	41.84	8.08	16.94	19.91	13.46	22.84	31.04
N (wt%)	0	0	0.36	0.62	0.96	0.99	1.44	1.32	0.84	0.53

Figure 7A and B presents a cross-sectional view of the hole in group G. The bottom side was the base layer, and the top side was the passivated layer (Figure 7A). The cross section of the zinc layer was still attached to the molybdate passivation, which can prove that the formation of holes were in the passivation layer of Na₂MoO₄. Figure 7B is a partial enlarged view of the mixture film in Figure 7A. A certain amount of the benzimidazole was adsorbed at the surface of the zinc layer at the holes. It can block the penetration of the corrosive medium and reduce the corrosion rate. The compound inhibitor was attached to a relatively small active point area judging from the appearance of the HDGS coupons.

Figure 7:

FESEM of active point pits of HDGS in group G.

The composition of substances was analyzed by XRD (Figure 8), which were immersed in simulated seawater of groups A, B, C and G, respectively. The corrosion product of HDGS in group A was ZnO (PDF code: 36-1451). There was only Fe and Zn in group B, because MoO₄²⁻ was binding Zn²⁺, which was dissociated from HDGS coupons. Organic elements such as C and N were found in group C, the Zn(N₃)₂, especially. The outermost electron of N in benzimidazole bound to Zn²⁺ to form a film (Ramakrishnan et al. 2022; Wang et al. 2021). There were also peaks of C, N and Zn(N₃)₂ in group G and the peak intensities were more than that in group C, indicating that the passivation behavior played a role in assisting the adsorption.

Figure 8:

XRD pattern of corrosion inhibitor film on HDGS.

Figure 9 presents a schematic diagram of the compound inhibitor. When the HDGS coupons were immersed in simulated seawater, the zinc layer initially played an electrochemical protective role, while Zn lost electrons and became Zn²⁺. Subsequently, MoO₄²⁻ combined with Zn²⁺ to form passivation layer. But the Cl⁻ of the simulated seawater attacked passivation layer to form defects such as gaps and holes. At this time, the benzimidazole came close to the substrate due to the charge factor, combining the free electrons and adsorbing at the defects. Hence, a passivation-adsorption composite film formed eventually.

Figure 9:

Working principle of compound inhibitor.

3.3 Performance test of composite WPUC

Figure 10 shows the change curves of corrosion area of WPUC with and without compound inhibitor in simulated seawater. The corrosion area of the WPUC with compound inhibitor expanded much more slowly than the WPUC without compound inhibitor. The visual corrosion area of the WPUC was fully covered at 192 h, while that of the WPUC with compound inhibitor was only 47%. It proved that the compound inhibitor work whether it was added to the corrosive medium directly or into the coating.

Figure 10:

Curves of corrosion area of WPUC with and without compound inhibitor in simulated seawater with different immersion times.

Figure 11 presents the curves of the impedance changes of the WPUC with and without compound inhibitor in simulated seawater at 25 °C with time. After immersion for 12 h, the impedance of both coatings dropped rapidly, which was caused by the dissolution of the coatings in seawater solution (Agnol et al. 2021). The impedance of WPUC with compound inhibitor was slightly lower than that of the WPUC without compound inhibitor. Because Na₂MoO₄, as an inorganic salt, increased the water solubility of the coating. In the dissolution process of coating, the infiltration of corrosive medium made the compound inhibitor come into work. After 24 h, the passivation adsorption process was completed and a composite film was formed to work with the polyurethane coating together. The impedance of WPUC with compound inhibitor kept higher than that of the WPUC without compound inhibitor at the following times. When the impedance dropped to 2 kΩ·cm² in the pre-experiment, the coating failed completely. The impedance of the WPUC without compound inhibitor dropped to 2 kΩ·cm² at 240 h, while the impedance of the composite coating still was 5 kΩ·cm² at 400 h. The results of corrosion area and impedance change were consistent. The compound inhibitor can prolong the service life of the WPUC by one time.

Figure 11:

Curves of the impedance of the different WPUC/ HDGS in simulated seawater with different immersion times.

4 Conclusions

The influence of sodium molybdate & benzimidazole binary compound corrosion inhibitor on the corrosion behavior of HDGS in the marine environment was studied in this paper. It was found that the corrosion inhibition efficiency was the highest of 99.62% when the total content was 1 wt% and the ratio of Na₂MoO₄ and benzimidazole was 9:1. Under this condition, the corrosion current density was 5.65 × 10⁻⁸ A/cm², while that of HDGS in simulated seawater without compound inhibitor was 1.483 × 10⁻⁵ A/cm². The principle of the compound inhibitor was that Na₂MoO₄, as a passivation type corrosion inhibitor, bounded Zn at the active sites of HDGS and created structural defects. Benzimidazole, as an adsorption type corrosion inhibitor, was attracted by electricity and adsorbed at the structural defects. The addition of the compound inhibitor could cause defects in WPUC and a small decrease of corrosion resistance initially. The corrosion inhibitor then worked during the corrosion process to make more than double the service life of WPUC.

Corresponding author: Chengfei Zhu, College of Materials Science and Engineering, Nanjing Tech University, 30 South PuZhu Road, Nanjing, Jiangsu211800, PR China, E-mail: Njtechzhucf@163.com

Funding source: National Natural Science Foundation of China

Award Identifier / Grant number: 21203095

Funding source: Jiangsu National Synergetic Innovation Center for Advanced Materials

Funding source: Priority Academic Program Development of Jiangsu Higher Education Institutions

Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.
Research funding: This study was supported by the National Natural Science Foundation of China (grant no. 21203095), the Jiangsu National Synergetic Innovation Center for Advanced Materials (SICAM) and the Priority Academic Program Development of Jiangsu Higher Education Institutions.
Conflicts of interest: The authors declare that they have no conflicts of interest regarding this article.

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Received: 2022-05-23

Accepted: 2022-12-31

Published Online: 2023-01-23

Published in Print: 2023-04-25

Artikel in diesem Heft

https://doi.org/10.1515/corrrev-2022-0043

Schlagwörter für diesen Artikel

hot-dip galvanized steel; marine environment; sodium molybdate compound corrosion inhibitor; waterborne polyurethane