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Repassivation characteristics of carbon steel in chloride-free pore solution after thermal cycles of simulated tropical marine environments

  • Tong Wu ORCID logo , Xingguo Feng ORCID logo EMAIL logo , Xiangyu Lu , Ning Zhuang and Shuai Qu
Published/Copyright: March 18, 2024
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Corrosion Reviews
From the journal Corrosion Reviews Volume 42 Issue 3

Abstract

Repassivation characteristics of carbon steel experienced thermal cycles in tropical marine environments were investigated in a simulated concrete pore solution (SCPS). The results suggested that the damage of passive films on the carbon steel mainly occurred during the cooling process in thermal cycles. The damaged passive films gradually recovered in the SCPS, and the duration of repassivation extended with the amplitude of thermal cycles and cyclic number in the high-amplitude thermal cycles (20–60 °C and 20–70 °C), while it was not significantly affected by the cyclic number in the low-amplitude thermal cycles (20–40 °C and 20–50 °C).

Keywords: repassivation; thermal cycle; passive film; buckling

1 Introduction

Tropical marine climate is characterized by abundant rainfall and large temperature difference between day and night. The daily average temperature may exceed 40 °C and the peak values are much higher (Gastaldi and Bertolini 2014). Therefore, the degradation of reinforced concrete serving in the tropical marine climate was extremely significant due to the high temperature and its high-amplitude temperature change. In the past several decades, much attention has been paid to the effect of temperature on the corrosion behavior of reinforcements in concrete environments. Liu and Weyers (1998) established a non-linear regression model, and their model demonstrated that there was a functional relationship between the corrosion rate of steel and temperature in concrete. When the temperature increased from 5 °C to 35 °C, the corrosion rate of rebar became threefold, which changed from ∼1.1 μA cm−2 to 3.4 μA cm−2 in the concrete containing a concentration of 1.8 kg m−3 water-soluble chloride. Similarly, a mathematical model developed by Pour-Ghaz et al. (2009a,b) also indicated that the corrosion rate of steel increased with the temperature in concrete. However, the increment of the corrosion rate was not as dramatic as reported by Liu and Weyers (1998). The corrosion rate of reinforcement only increased by 20 % when the temperature increased from 10 °C to 50 °C (Pour-Ghaz et al. 2009a,b). Baccay et al. (2006) investigated the influence of temperature on the corrosion behavior of steel rebars in carbonated concrete, and they reported that the corrosion rate of the rebar was accelerated by the increase of temperature. Hussain et al. (1995) studied the threshold chlorides of reinforcements in concrete pore solution at different temperatures. The results suggested that the threshold chlorides reduced from 1 % to 0.19 % by weight of cement, when the temperature increased from 20 °C to 70 °C. Dong et al. (2020) investigated the corrosion behavior of reinforcements in a chloride-contaminated concrete pore solution at various temperatures. The authors noticed that the charge transfer resistance of the carbon steel decreased from 15.9 kΩ cm2 to 8.8 kΩ cm2, and its corrosion current density increased from 0.96 μA cm−2 to 6.74 μA cm−2 as the temperature changed from 25 °C to 55 °C. Similarly, Liu et al. (2021) studied the corrosion rate of carbon steel in SCPS at different temperatures by potentiodynamic polarization and Tafel analysis. Their results showed that the corrosion current density of the carbon steel increased from 0.42 μA cm−2 to 4.5 μA cm−2, when the temperature increased from 25 °C to 80 °C. An earlier study carried out by Gastaldi and Bertolini (2014) also indicated that rebars presented higher corrosion current density and more negative corrosion potential in the higher temperature environment. Qiu et al. (2020) conducted experiments to investigate the corrosion characteristics of carbon steels at various temperatures in anoxic SCPS. Their results revealed that the polarization resistance decreased while the passive film thickness increased with the increasing temperature. The authors attributed this situation to the higher density of defects in the passive film at a higher temperature. In summary, it is generally accepted that the high temperature has an adverse effect on the corrosion of reinforcements in concrete environments, and the quantitative relation between corrosion rates of rebar and environment temperatures should be further investigated.

In fact, the temperature varies over a wide range and changes frequently in tropical marine climate environments. It is important to investigate the impact of temperature change on durability of concrete structures in the tropical marine climate. Our earlier studies (Feng et al. 2020; Wu et al. 2022) researched the passive behavior of carbon steel and stainless steel under alternating temperature conditions. It was found that passive films on both carbon steels and stainless steels were damaged by the temperature alternation. The polarization resistance of the steel samples decreased with the amplitude and frequency of temperature change, and the passive film cracked after experiencing high amplitude of temperature change. However, the repassivation behavior of the reinforcements that experienced temperature alternations was not reported in previous studies (Feng et al. 2020; Wu et al. 2022).

Repassivation behavior of reinforcement in different environments also attracted a great deal of attention. Carvalho et al. (2022) studied the repassivation of reinforcement which was corroded for different times in SCPS. The authors found that the solution with a higher pH was more conducive to the repassivation of reinforcement. Meanwhile, the severely corroded reinforcement, which was corroded for 28 days, was difficult to repassivate in the SCPS. Zajec et al. (2022) recorded the current transients and the coupled potential of steel when it was scratched in a neutral solution, and they noticed that the charge for repassivation mainly came from the double layer capacitance of passive films, rather than from the cathodic reactions. Then, the authors deduced that a scratch on a large-area electrode was easier to repassivate, compared to that on a small electrode, since the double layer capacitance depends on the area. Jun et al. (2020) studied the repassivation behaviour of pitting on Super 13Cr stainless steel in 85 °C NaCl solution. They reported that the pitting could repassivate only when the potential was below a cutoff potential (for S13Cr pits at 85 °C in 0.3 M NaCl, this value was close to −0.27 VSCE) during potentiostatic polarization, and the repassivation time was shorter at a lower potential. Feng et al. (2016) paid attention to the growth and repassivation of metastable pitting on deformed 304 stainless steel in a simulated pore solution. The results suggested that the growth rate of metastable pitting was slightly affected by the magnitude of deformation, while the repassivation rate of metastable pitting was significantly decreased by the magnitude of deformation.

The repassivation characteristic of steel rebars can affect pitting initiation and development, and it is one of the key factors for the durability of concrete structures. Unfortunately, the repassivation behavior of rebars, which experienced temperature change in tropical marine environments, has not been investigated. In the present study, the repassivation characteristics of carbon steels experienced different thermal cycles were studied in SCPS. The results suggested that the damage of passive films mainly occurred during the cooling stage in the thermal cycles, and the duration of repassivation was closely related to the amplitude and the cyclic number of thermal cycles.

2 Materials and methods

2.1 Materials

Carbon steels with chemical composition of 0.37 % C, 0.16 % Si, 0.32 % Mn, 0.053 % S, 0.026 % P, and 99.071 % Fe were adopted to investigate the repassivation behavior after different thermal cycles. The carbon steel sample with a size of Φ10 × 10 mm was used in the present study. A copper wire was welded on one end of the cylindrical carbon steel. Then, the sample was coated with epoxy resin, and only the other end was exposed for electrochemical testing. The exposed end was ground with emery paper No. 800, and degreased and douched by applying absolute ethyl alcohol and deionized water, respectively, before experiments. A synthetic solution, which contained 0.027 M Ca(OH)2, 0.25 M KOH, and 0.25 M NaOH, was used to simulate the concrete pore solution (Adewumi et al. 2021). The pH of the SCPS was 13.5 at 20 °C and 13.2 at 70 °C. The decrease in pH is mainly caused by ionization, and it was ignored in the present study.

2.2 Experimental procedures

Thermal cycles were performed by a homemade apparatus shown in Figure 1. Initially, the prepared carbon steels were immersed in 20 °C SCPS for 48 h so that the samples could finish passivation, according to our previous study (Wu et al. 2022). Then, the pump connecting to the hot SCPS was turned on and the hot solution was continuously pumped into the inner layer of the apparatus. The temperature of the SCPS increased rapidly and reached the design high temperature in 10–15 min, and then the solution temperature was maintained at a high value for 1 h. Afterward, the pump for the hot SCPS was turned off and another pump connecting to the cooling water was turned on automatically, and the cooling water was pumped into the outer layer of the apparatus for 3 h, and the temperature of the SCPS decreased to 20 °C. Thus, one thermal cycle of the SCPS finished. Temperature change of the designed thermal cycles is presented in Figure 2. For investigating the effect of the amplitudes and cyclic number of the thermal cycle on the repassivation behavior of the carbon steel in the SCPS, thermal cycles including 20–40 °C, 20–50 °C, 20–60 °C, and 20–70 °C cycles, and each thermal cycle with 1 time, 5 times, 10 times, 15 times, and 20 times, were performed, respectively.

Figure 1: Illustration of the homemade thermal cycle apparatus.
Figure 1:

Illustration of the homemade thermal cycle apparatus.

Figure 2: Temperature variation of the experimental thermal cycles in the SCPS.
Figure 2:

Temperature variation of the experimental thermal cycles in the SCPS.

After the carbon steels experienced different thermal cycles, the samples were maintained in 20 °C SCPS, and electrochemical measurements were tested at 1 h, 2 h, 4 h, 6 h, 8 h, and 24 h in the SCPS at 20 °C to investigate the repassivation characteristics. The carbon steel sample, an Ag/AgCl (saturated KCl) electrode, and a platinum plate were connected to the working electrode (WE), reference electrode (RE), and counter electrode (CE), respectively. Three parallel specimens were tested, and the mean values or middle curves were used to represent the electrochemical results of the carbon steel experiencing different thermal cycles. The open circuit potential (OCP) was measured until the change was less than 5 mV in 10 min. Linear polarization tests were performed from −10 mV to +10 mV versus OCP at a sweep rate of 0.1667 mV/s (Carvalho et al. 2022). Electrochemical impedance spectroscopy (EIS) measurements were carried out by applying a 10 mV AC disturbance signal, with a frequency range between 105 and 10−2 Hz. For acquiring the range of passivation potentials of the carbon steel samples, potentiodynamic polarization curves were measured after the samples were immersed in different temperature SCPS for 2 h. The potentiodynamic polarization tests were initiated from OCP and ended as the anodic current density was higher than 0.1 mA/cm2 at a sweep rate of 1 mV/s (Feng et al. 2018; Feng et al. 2019; Li et al. 2021). Obvious passive ranges were observed in the polarization curves when the potentials were in the range of 0.3–0.4 VAg/AgCl. Thus, the samples were potentiostatically polarized at 0.3 VAg/AgCl, and the current transients were recorded, when the samples experienced thermal cycles, for investigating its repassivation characteristics. Furthermore, the surface morphologies of the carbon steels were observed by applying a JSM7800F scanning electron microscope (SEM) after different thermal cycles.

3 Results and discussion

3.1 Open circuit potential

The OCP of carbon steel samples is presented in Figure 3, after different amplitudes of thermal cycles. The OCP of the carbon steel was in the range of −140 to −120 mV, after 48 h of immersion in the SCPS at 20 °C, suggesting complete passivation of the carbon steel (ASTM 2015) in the initial stage. After experiencing thermal cycles, the OCP values of the samples obviously decreased with the amplitudes of the thermal cycles. For instance, as shown in Figure 3a, the OCP of the samples experienced one time 20–40 °C thermal cycle and showed no significant change compared with that of the passivated one, while that of its counterpart, which experienced one time 20–70 °C thermal cycle, sharply dropped to −220 mV. As the cyclic number of the thermal cycles increased to ten times (Figure 3b), the OCP of the former sample did not obviously further decrease, while that of the latter one dropped to −250 mV. This situation indicated that the decrease of the OCP was aggravated by the cyclic number in the high-amplitude thermal cycles (20–70 °C cycles), while that of its counterpart was not significantly affected by the cyclic number in the low-amplitude thermal cycles (20–40 °C cycles). Our previous studies (Feng et al. 2020; Wu et al. 2022) suggested that the decrease of the OCPs can be attributed to the formation of cracks in the passive film in the chloride-free pore solution.

Figure 3: OCPs of carbon steel samples in SCPS under different thermal cycles: (a) one time of thermal cycle and (b) ten times of thermal cycles.
Figure 3:

OCPs of carbon steel samples in SCPS under different thermal cycles: (a) one time of thermal cycle and (b) ten times of thermal cycles.

In the repassivation stage, the OCPs of the carbon steels gradually increased and finally reached the OCPs of passivated samples, indicating the complete repassivation of the carbon steel samples. Furthermore, the duration of repassivation of the carbon steel extended with the amplitudes of the thermal cycles, as well as the cyclic number in the high-amplitude thermal cycles. As shown in Figures 3 and 4, for the carbon steel experienced the low-amplitude thermal cycle (20–40 °C and 20–50 °C), its repassivation finished in 4 h, and the time did not increase with the cyclic number. However, for the samples that experienced the high-amplitude thermal cycles (20–70 °C), the repassivation time extended to about 8 h after one time thermal cycle, and the ones experienced 20 times high-amplitude thermal cycles even could not finish repassivation in 24 h (Figure 4c).

Figure 4: OCPs of carbon steel samples experienced different cyclic numbers of thermal cycles: (a) 20–40 °C thermal cycles, (b) 20–60 °C thermal cycles, and (c) 20–70 °C thermal cycles.
Figure 4:

OCPs of carbon steel samples experienced different cyclic numbers of thermal cycles: (a) 20–40 °C thermal cycles, (b) 20–60 °C thermal cycles, and (c) 20–70 °C thermal cycles.

3.2 Linear polarization resistance

Linear polarization resistance (Rp) of the carbon steel was calculated from the slope of the linear polarization plots. Rp of the carbon steel samples experienced different thermal cycles are presented in Figures 5 and 6. Obviously, the value of Rp slightly decreased after various cyclic numbers in the low-amplitude thermal cycles (20–40 °C), while those of its counterparts dramatically decreased for the ones that experienced the high-amplitude thermal cycles (20–60 °C, 20–70 °C). Furthermore, the duration of Rp increased, which represents the repassivation of the carbon steel sample, extended with the amplitude of temperature change and the cyclic number in the high-amplitude thermal cycles. Approximately 8 h was taken to finish the repassivation for the sample experienced one time 20–70 °C thermal cycle, and the time was prolonged to more than 24 h as the cyclic number reached 20 times under the same thermal cycles (Figure 6c). However, the repassivation time was only about 4 h for the sample experienced one time low-amplitude thermal cycle (20–40 °C and 20–50 °C), and it did not evidently change with the cyclic number (Figures 5b and 6a). This situation is consistent with the OCP results, which suggests that the repassivation time of the carbon steel extended with the amplitude of thermal cycles, as well as the cyclic number in the high-amplitude thermal cycles (20–60 °C, 20–70 °C) in the chloride-free SCPS. In comparison, the duration of repassivation was not significantly affected by the cyclic number, for the sample experienced the low-amplitude thermal cycles (20–40 °C and 20–50 °C).

Figure 5: Linear polarization resistance of carbon steel samples in the SCPS under different amplitudes of thermal cycles: (a) one time of thermal cycles and (b) ten times of thermal cycles.
Figure 5:

Linear polarization resistance of carbon steel samples in the SCPS under different amplitudes of thermal cycles: (a) one time of thermal cycles and (b) ten times of thermal cycles.

Figure 6: Linear polarization resistance of carbon steel samples experienced different cyclic numbers of thermal cycles: (a) 20–40 °C thermal cycles, (b) 20–60 °C thermal cycles, and (c) 20–70 °C thermal cycles.
Figure 6:

Linear polarization resistance of carbon steel samples experienced different cyclic numbers of thermal cycles: (a) 20–40 °C thermal cycles, (b) 20–60 °C thermal cycles, and (c) 20–70 °C thermal cycles.

3.3 Electrochemical impedance spectroscopy

Figure 7 displays the electrochemical impedance spectroscopy of the carbon steel samples experienced different thermal cycles. Generally, the radius of the arc in Nyquist plots and the impedance in Bode plots obviously decreased after thermal cycles, indicating the crack of the passive film. As the immersion time increased, the repassivation of the passive film cracked sample gradually progressed, and the radius of arc at low frequency increased. For samples experienced the low-amplitude thermal cycle (20–40 °C), its radius at low frequency could grow to the value of the passivated samples in 4 h. In comparison, for the counterparts experienced 10 times of high-amplitude thermal cycles (20–70 °C), the radius could not even reach the latter value after 24 h repassivation (Figure 7c and d).

Figure 7: The Nyquist plots and Bode plots of carbon steel samples in SCPS before and after thermal cycles: (a, b) 20–40 °C and 20–70 °C thermal cycles for one time, (c, d) 20–40 °C and 20–70 °C thermal cycles for 10 times.
Figure 7:

The Nyquist plots and Bode plots of carbon steel samples in SCPS before and after thermal cycles: (a, b) 20–40 °C and 20–70 °C thermal cycles for one time, (c, d) 20–40 °C and 20–70 °C thermal cycles for 10 times.

An equivalent circuit shown in Figure 8 was adopted to fit the experimental data of EIS (Feng et al. 2011a,b; Mohammadi et al. 2011; Sahoo and Balasubramaniam 2008), in which Rs is the solution resistance, Rf and Qf represent the resistance and capacitance of the passive film, respectively, Rct is the charge transfer resistance, and CPEdl is the double layer capacitance. In the present study, constant phase element (CPE) was used to substitute for pure capacitance (Feng et al. 2011a,b; Mohammadi et al. 2011; Sahoo and Balasubramaniam 2008), and the impedance of CPE (ZCPE) is given by Eq. (1):

(1)ZCPE=[Q(jw)n]−1

where n is the CPE exponent and w is the phase angle frequency. When n = 1, the CPE will be pure capacitance, and when n = 0, it will be pure resistance. This value of n is thought to be related to surface inhomogeneity and roughness (Cox and Wong 1995). The fitting results are shown in Figure 9 (fitting data id listed in Appendix 1).

Figure 8: Equivalent circuit for modeling the EIS data.
Figure 8:

Equivalent circuit for modeling the EIS data.

Figure 9: The fitted electrochemical parameters of carbon steel samples in SCPS before and after thermal cycles: (a) passive film resistance, (b) passive film capacitance, (c) charge transfer resistance, and (d) double layer capacitance.
Figure 9:

The fitted electrochemical parameters of carbon steel samples in SCPS before and after thermal cycles: (a) passive film resistance, (b) passive film capacitance, (c) charge transfer resistance, and (d) double layer capacitance.

As can be seen, Rf and Rct decreased, while Qf and CPEdl increased after the passivated steel experienced thermal cycles. The decrement of Rf and Rct, as well as the increment of Qf and CPEdl, increased with the amplitude of thermal cycles. As the repassivation of the carbon steel progressed, the aforementioned electrochemical parameters (Rf, Rct, Qf, CPEdl) gradually changed to their initial value, and most of the steel samples could finish repassivation in 24 h. In addition, the time of the repassivation of these carbon steel samples extended with the amplitude of thermal cycles and the cyclic number, especially in the high-amplitude thermal cycles. For instance, Rf and Qf slightly decreased after experiencing low-amplitude thermal cycles (20–40 °C), and the two parameters quickly recovered (less than 4 h) to their initial levels, regardless of the cyclic number. In comparison, the counterparts experienced one time high-amplitude thermal cycles (20–60 °C and 20–70 °C) took about 6–8 h to recover to their initial levels, while those of the ones experienced 20 times 20–60 °C and 20–70 °C cycles took more than 8 h and 24 h to the initial levels. Therefore, the fitting EIS results (Figure 9), together with OCP (Figures 3 and 4) and linear polarization resistance results (Figures 5 and 6), confirmed that the repassivation time of the carbon steel extended with the amplitude of thermal cycles and the cyclic number in the high-amplitude thermal cycles (20–60 °C and 20–70 °C). However, the repassivation time of the carbon steel did not show significant extension by the cyclic number in the low-amplitude thermal cycles (20–40 °C).

3.4 Current transients during thermal cycles

Current transient of the carbon steel, which was polarized at a passivation potential in the SCPS experienced a thermal cycle and then maintained at 20 °C, was recorded for investigating its repassivation characteristic. For acquiring the passivation potential of the carbon steel, potentiodynamic polarization curves were tested at different temperatures in the SCPS, and the results are presented in Figure 10. It is easy to notice that the carbon steel samples were in the passive state in the range between 0.3 and 0.4 VAg/AgCl. Then, carbon steel samples were potentiostatically polarized at 0.3 VAg/AgCl in the SCPS, and the current transients and the temperature changes were recorded during the thermal cycles (Figure 11). In these thermal cycles, the heating stage began at 240 min and rapidly rose to these design high temperatures in 10–15 min. Subsequently, the temperature of the SCPS was maintained at these high values for about 10 min. Thereafter, the temperature quickly dropped to 20 °C in 10–15 min and then maintained at 20 °C. Obviously, the current density of the carbon steel sharply increased with the temperature in these thermal cycles, which indicates that the stability of the passive film decreased with increasing temperature. Many current peaks, which were ascribed to the cracks of passive films according to previous studies (Feng et al. 2016, 2020; Wu et al. 2022), were observed in these current transients. Furthermore, more peaks were noticed during the temperature drop period than the temperature rise period in the same thermal cycle, especially for the samples experienced the high-amplitude thermal cycles. This situation suggests that the damage of passive films on the carbon steel mainly occurred during the temperature drop period in thermal cycles. The duration of the repassivation, corresponding to the time for the current density declining to its initial value before temperature change, significantly extended with the amplitude of thermal cycles. For instance, the current density declined to its initial value in 10 min when the temperature dropped from 40 °C to 20 °C, while that of the counterpart took around 55 min when the SCPS temperature dropped from 70 °C to 20 °C. This scenario was consistent with the repassivation time results exhibited in the OCPs (Figures 3 and 4), linear polarization resistance (Figures 5 and 6), and electrochemical impedance spectroscopy (Figure 9).

Figure 10: Potentiodynamic polarization curves of carbon steel samples in SCPS at different temperatures.
Figure 10:

Potentiodynamic polarization curves of carbon steel samples in SCPS at different temperatures.

Figure 11: Current transients of carbon steel samples polarized at 0.3 VAg/AgCl during thermal cycles with different amplitudes.
Figure 11:

Current transients of carbon steel samples polarized at 0.3 VAg/AgCl during thermal cycles with different amplitudes.

3.5 Surface morphology of repassivation carbon steel

Figure 12 shows the surface morphologies of carbon steel samples experienced different thermal cycles and repassivation situation. For the sample that experienced low-amplitude thermal cycles (20–40 °C), no obvious defect, except for a micro-crack, was observed on the surface even if the sample experienced 20 times of thermal cycle (Figure 12a). In comparison, typical buckling can be observed on the surface when the counterpart experienced a single time of high-amplitude (20–70 °C) thermal cycle (Figure 12b). As the cyclic number of the high-amplitude thermal cycle increased to 20 times, more significant damage existed on the surface, where the buckling passive film fractured and stripped from the substrate (Figure 12 c). This situation suggests that the damage of the passive films was not aggravated by the increasing cyclic in the low-amplitude thermal cycles, while that was dramatically intensified by the increasing cyclic in the high-amplitude thermal cycles.

Figure 12: Surface morphologies of canbon steel experienced different thermal cycles and the surface morphologies during the repassivation process: (a) repassivated for 1 h in 20 °C SCPS after experiencing 20 times of 20–40 °C thermal cycles, (b) repassivated for 1 h in 20 °C SCPS after experiencing a single time of 20–70 °C thermal cycles, (c) repassivated for 1 h in 20 °C SCPS after experiencing 20 times of 20–70 °C thermal cycles, (d) repassivated for 4 h in 20 °C SCPS after experiencing a single time of 20–70 °C thermal cycles, and (e) repassivated for 8 h in 20 °C SCPS after experiencing a single time of 20–70 °C thermal cycles, (f) repassivated for 24 h in 20 °C SCPS after experiencing 20 times of 20–70 °C thermal cycles.
Figure 12:

Surface morphologies of canbon steel experienced different thermal cycles and the surface morphologies during the repassivation process: (a) repassivated for 1 h in 20 °C SCPS after experiencing 20 times of 20–40 °C thermal cycles, (b) repassivated for 1 h in 20 °C SCPS after experiencing a single time of 20–70 °C thermal cycles, (c) repassivated for 1 h in 20 °C SCPS after experiencing 20 times of 20–70 °C thermal cycles, (d) repassivated for 4 h in 20 °C SCPS after experiencing a single time of 20–70 °C thermal cycles, and (e) repassivated for 8 h in 20 °C SCPS after experiencing a single time of 20–70 °C thermal cycles, (f) repassivated for 24 h in 20 °C SCPS after experiencing 20 times of 20–70 °C thermal cycles.

Damage of the passive film on the carbon steel caused by the thermal cycles should be related to the thermal stress, as illustrated in Figure 13. When the carbon steel experienced the heating stage of thermal cycles, the theoretical thermal expansion of the substrate was larger than that of the passive film for their different thermal expansion coefficients (carbon steel substrate, 16 × 10−6/K; passive film, 13 × 10−6/K (Polanco et al. 2004; Yang et al. 2017)). Then, mismatch stress will occur at the film/substrate interface, and the passive film will bear thermal tensile stress. The thermal tensile stress in the passive film can be given by Eq. (2) (Schütze et al. 2006):

(2)σtherm=Ef1−νfεtherm=Ef1−νfΔT(αmet−αf)

where σtherm is the thermal tensile stress, εtherm is the thermal strain, Ef is the elastic modulus of the passive film, νf is the Poisson’s ratio of the passive film, ΔT is the temperature change of the SCPS, and αmet and αf are the thermal expansion coefficient of the carbon steel substrate and the passive film, respectively. It can be concluded that the thermal tensile stress is proportional to the amplitude of SCPS temperature change, according to Eq. (2). When the amplitude of temperature change exceeds a certain value, the thermal tensile stress can reach the yield strength of the passive film, and cracks occurred on the surface, as shown in Figure 13a. Simultaneously, passive films may locally debond from the carbon steel substrate during the heating stage (Figure 13b) (Freund and Suresh 2004). As the sample experiences the cooling stage of thermal cycles, the debonded passive film and the substrate will shrink, and the debonded passive film will suffer thermal compressive stress for its lower thermal expansion coefficient (Polanco et al. 2004; Yang et al. 2017). As a result, buckling will form in the debonded passive film under the thermal compressive stress (Figure 13c). According to Freund and Suresh (2004), the buckling film will fracture if the thermal compressive stress exceeds the critical value σcr, as illustrated in Figure 13d,

(3)σcr=π2Ef12(1−νf2)(hfam)2

where hf is the thickness of the passive film and am is the half width of the debonded zone. The current transient in Figure 11 exhibited more current peaks during the temperature drop periods in the thermal cycles. Surface morphologies in Figure 12b and (c) showed that the damage of passive films mainly came from the fracture of the buckling passive film after thermal cycles. The current transient results (Figure 11), together with the surface morphologies (Figure 12b and c), confirmed that the fracture of passive films on the carbon steel mainly occurred during the cooling stage in the thermal cycles in the SCPS.

Figure 13: Illustration of de-passivation and repassivation process of carbon steel after different thermal cycles: (a) cracks formed in the heating stage, (b) debond formed in the heating stage, (c) buckling formed in the cooling stage, (d) fracture buckling passive film, (e) the de-passivated film, and (f) repassivation of the damaged passive film.
Figure 13:

Illustration of de-passivation and repassivation process of carbon steel after different thermal cycles: (a) cracks formed in the heating stage, (b) debond formed in the heating stage, (c) buckling formed in the cooling stage, (d) fracture buckling passive film, (e) the de-passivated film, and (f) repassivation of the damaged passive film.

Carbon steel samples after different thermal cycles were maintained in 20 °C SCPS for repassivation. As the morphologies results (Figure 12d–f) show, the defects in the passive film gradually declined as the repassivation progressed. The duration of the repassivation obviously extended with the cyclic number in the SCPS with a high-amplitude thermal cycle (20–70 °C). The repassivation finished in 8 h (Figure 12e) for the sample experienced a single time of 20–70 °C thermal cycle, while that of the counterpart experienced 20 times of the same thermal cycle cannot finish in 24 h (Figure 12 f). This situation is consistent with the electrochemical results (Figures 4, 6, 9, and 11), confirming that the repassivation time of the carbon steel was extended by the amplitude of thermal cycles and cyclic number in the high-amplitude thermal cycles (20–60 °C and 20–70 °C). In comparison, the duration of repassivation was not significantly affected by the cyclic number for the ones in the SCPS experienced the low-amplitude thermal cycles (20–40 °C and 20–50 °C).

3.6 Repassivation characteristics after thermal cycles in SCPS

Electrochemical measurements and surface morphology results confirmed that passive films on the carbon steel were damaged by the high-amplitude thermal cycles (20–60 °C and 20–70 °C) in the SCPS. Furthermore, the current transient results and the surface morphology (Figure 12b and c) suggested that the damage of passive films mainly came from the fracture of the buckling zone during the cooling stage in thermal cycles. This scenario could be ascribed to the defects in the passive film. According to the point defect model (PDM) (Ahn et al. 2005; Cheng et al. 2002; Macdonald et al. 1992; Macdonald 1992, 1999), the passive film on the carbon steel was heavily doped, which contains numerous donor and cation vacancies (Macdonald et al. 1992; Macdonald 1992). The cation vacancy is inclined to concentrate at the film/substrate interface, and these concentrated cation vacancies debonded the passive film from the substrate (Macdonald et al. 1992; Macdonald 1992). As the steel sample experienced the low-amplitude thermal cycles in the SCPS, the thermal tensile stress caused by the temperature change ΔT did not exceed the yield strength of the passive film. Thus, the electrochemical parameters, such as OCP, linear polarization resistance, and passive film resistance, did not show significant change after the low-amplitude thermal cycles. These electrochemical parameters slightly changed, and a few micro-cracks were observed in the passive film (Figure 12a), after experiencing low-amplitude thermal cycles. The slight change in the electrochemical parameters could be ascribed to the local cation vacancy condensation, according to the PDM (Ahn et al. 2005; Cheng et al. 2002; Macdonald et al. 1992; Macdonald 1992, 1999). Similarly, when the carbon steel sample experienced the high-amplitude thermal cycles, the passive film was preferentially damaged in the cation vacancy condensated and debonded zone. Especially, buckling and fracture were easy to occur in the debonded passive film during the cooling stage in the thermal cycles. As a result, as Figures 11 and 12 showed, the damage of the passive film on the carbon steel was mainly observed during the cooling stage of thermal cycles in the SCPS.

The electrochemical measurements (Figures 3, 5–7 and 11) and surface morphology results (Figure 12a–c) suggested that the duration of repassivation was extended by the increasing cyclic number of the high-amplitude thermal cycles (20–60 °C, 20–70 °C), as well as the increasing amplitude of thermal cycles. However, the duration of repassivation was not significantly affected by the cyclic number when the sample experienced the low-amplitude thermal cycles (20–40 °C, 20–50 °C). According to the PDM (Macdonald et al. 1992; Macdonald 1992, 1999), during the repassivation of the carbon steel in the SCPS, a new passive film grew at the metal/film interface while the film simultaneously dissolved at the film/solution interface. In the present study, the carbon steels were initially passivated in 20 °C SCPS, and the samples were maintained in the same solution for repassivation after different thermal cycles. During their repassivation process, it is reasonable to assume that the passive film growth rate at the metal/film interface and its dissolution rate at the film/solution interface were identical for the samples experienced different thermal cycles. While the film growth rate was identical, the damage caused by high-amplitude thermal cycles was more serious than that caused by low-amplitude thermal cycles, and the damage could accumulate as the sample went through one high-amplitude thermal cycle after another. Therefore, as the cyclic number of high-amplitude thermal cycles increased, the damage in the passive film gradually accumulated and expanded. As shown in Figure 13e and f, the complete repassivation of the carbon steel means the elimination of the damage in the passive film, and the duration of the damage elimination process will be extended by the increasing film damage degree. As a result, the repassivation time extended with the amplitude of thermal cycles and the cyclic number in the high-amplitude thermal cycles (20–60 °C and 20–70 °C). In comparison, the damage caused by low-amplitude thermal cycles was less serious and could be healed before the next cycle. Thus, the damage will not accumulate when the steel goes through several low-amplitude thermal cycles. As a result, the repassivation time was not significantly affected by the cyclic number when the samples experienced the low-amplitude thermal cycles (20–40 °C, 20–50 °C). In general, the carbon steels could finish repassivation in 4 h in 20 °C SCPS, after the samples experienced different times of the low-amplitude thermal cycles (20–40 °C, 20–50 °C), as shown in Figures 3, 4–6 and 9. For the samples that suffered the high-amplitude thermal cycles (20–60 °C, 20–70 °C), the duration of the repassivation was ∼ 8 h and more than 24 h when the samples experienced one time and 20 times of thermal cycles (Figures 3, 4–6, 9 and 12), respectively.

4 Conclusions

  1. The OCP value, linear polarization resistance (Rp), passive film resistance (Rf), and charge transfer resistance (Rct) of the carbon steel decreased, while the passive film capacitance (Qf) and double layer capacitance (CPEdl) of samples increased, with the increasing amplitude of thermal cycles and the cyclic number of the high-amplitude thermal cycles (20–60 °C and 20–70 °C). However, the aforementioned parameters of carbon steel did not show significant influence by the cyclic number in the low-amplitude thermal cycles (20–40 °C and 20–50 °C).

  2. After experiencing different thermal cycles, the carbon steel can repassivate in the 20 °C chloride-free SCPS. The duration of the repassivation of samples was not significantly affected by the cyclic number in the low-amplitude thermal cycles (20–40 °C and 20–50 °C), while that of the counterparts obviously extended with the amplitude of thermal cycles and the cyclic number in the high-amplitude thermal cycles (20–60 °C and 20–70 °C). In general, the carbon steel could repassivate in 4 h in the 20 °C SCPS, after experiencing the former thermal cycles, even if the steel suffered 20 times low-amplitude thermal cycles. For the samples experienced the latter thermal cycles, it would take ∼8 h and more than 24 h to repassivate for the steel experienced a single time and 20 times high-amplitude thermal cycles, respectively.

  3. When the carbon steels experienced the high-amplitude thermal cycles in the SCPS, the damage to passive films mainly occurred during the cooling stage in the form of buckling and the fracture of buckling film, and the damage was obviously aggravated by the increasing cyclic number. In comparison, the damage to the passive film was not significantly affected by the cyclic number for the counterparts that experienced the low-amplitude thermal cycles.

Corresponding author: Xingguo Feng, Key Laboratory of Coastal Disaster and Defence, Ministry of Education, College of Harbour, Coastal and Offshore Engineering, Hohai University, Nanjing, 210024, Jiangsu, China, E-mail:

Funding source: Fundamental Research Funds for the Central Universities

Award Identifier / Grant number: B230205023

Funding source: National Key Research and Development Program of China

Award Identifier / Grant number: 2022YFB3207400

  1. Research ethics: Not applicable.

  2. Author contributions: Conceptualization, Feng, X.G.; methodology, Wu, T., Qu, S.; software, Lu. X.Y.; validation, Wu, T.; formal analysis, Feng, X.G.; investigation, Wu, T.; resources, Feng, X.G.; data curation, Wu, T.; writing – original draft preparation, Wu, T.; writing – review and editing, Feng, X.G., Qu, S.; visualization, Lu. X.Y.; supervision, Zhuang, N.; project administration, Lu. X.Y.; funding acquisition, Feng, X.G. The authors have accepted responsibility for the entire content of this manuscript and approved its submission.

  3. Research funding: This work is supported by the National Key R&D Program of China (No. 2022YFB3207400) and the Fundamental Research Funds for the Central Universities (No. B230205023).

  4. Conflicts of interest: The authors declare that they have no conflicts of interest to this work.

  5. Data availability: The raw data can be obtained on request from the corresponding author.

Appendix 1: The fitting results of the EIS data are shown in Table A1

Table A1:

The fitted electrochemical parameters of carbon steels in SCPS before and after thermal cycles.

R s (Ω cm2) Q f ( × 10−7 F cm−2) R f (Ω cm2) CPE dl ( × 10−4 Ω−1 Sn cm−2) n R ct ( × 104 Ω cm2)
20–40 °C for 1 time Before 6.842 1.418 40.89 2.101 0.8494 22.73
1 h 6.524 1.436 39.25 2.141 0.8277 20.28
2 h 6.417 1.428 40.84 2.111 0.8245 21.24
4 h 6.737 1.422 40.61 2.102 0.8501 23.97
6 h 6.993 1.424 43.04 2.081 0.8362 23.96
8 h 6.742 1.422 41.93 2.086 0.8259 24.73
24 h 6.827 1.415 42.23 2.097 0.8126 25.44
20–40 °C for 10 times Before 5.866 1.480 40.33 2.193 0.8369 23.46
1 h 6.656 1.484 39.81 2.238 0.8418 20.15
2 h 6.093 1.489 41.05 2.196 0.8343 22.75
4 h 6.620 1.497 40.09 2.188 0.8230 23.60
6 h 6.215 1.503 40.53 2.132 0.8224 26.94
8 h 6.236 1.492 40.04 2.102 0.8495 28.00
24 h 6.855 1.486 40.53 2.099 0.7988 27.13
20–40 °C for 20 times Before 6.875 1.532 38.29 2.341 0.8523 17.14
1 h 6.698 1.588 37.19 2.395 0.8360 15.54
2 h 6.748 1.583 40.19 2.392 0.8441 15.35
4 h 6.688 1.553 38.64 2.336 0.8157 17.67
6 h 6.670 1.536 38.04 2.314 0.8216 18.93
8 h 6.802 1.504 39.55 2.309 0.8208 18.49
24 h 6.667 1.489 40.26 2.320 0.8072 17.80
20–50 °C for 1 time Before 7.688 1.304 41.83 2.190 0.8323 21.52
1 h 8.271 1.506 40.07 2.333 0.8297 15.50
2 h 8.426 1.474 39.24 2.296 0.8365 19.05
4 h 7.890 1.371 41.37 2.199 0.8331 21.64
6 h 7.905 1.294 42.17 2.173 0.7995 22.19
8 h 8.052 1.322 41.94 2.172 0.8140 22.00
24 h 8.022 1.258 42.79 2.161 0.8174 23.40
20–50 °C for 10 times Before 5.883 1.450 42.00 1.966 0.8518 22.55
1 h 5.612 1.686 40.60 2.158 0.8500 17.73
2 h 5.418 1.578 42.58 2.168 0.8367 19.23
4 h 5.330 1.432 41.23 2.113 0.8392 21.96
6 h 6.295 1.456 41.75 1.995 0.8412 23.03
8 h 6.202 1.448 41.60 1.951 0.8389 23.16
24 h 6.034 1.444 41.67 1.961 0.8277 23.78
20–50 °C for 20 times Before 8.601 1.394 44.17 2.070 0.8335 21.86
1 h 8.839 1.510 41.51 2.241 0.8558 16.02
2 h 9.063 1.502 41.63 2.155 0.8319 19.37
4 h 8.931 1.487 43.76 2.074 0.8206 21.93
6 h 9.239 1.355 44.80 2.064 0.7983 22.15
8 h 8.456 1.391 44.05 2.058 0.8148 22.26
24 h 9.043 1.332 44.45 2.032 0.8125 21.89
20–60 °C for 1 time Before 6.439 1.344 40.04 2.008 0.8381 19.81
1 h 6.229 1.700 35.14 2.294 0.8437 10.29
2 h 6.853 1.686 36.13 2.219 0.8163 11.39
4 h 6.992 1.485 37.87 2.196 0.8294 12.43
6 h 7.073 1.317 39.76 2.024 0.8420 19.32
8 h 6.904 1.379 39.87 1.954 0.8010 19.66
24 h 7.229 1.374 39.84 1.961 0.7874 19.80
20–60 °C for 10 times Before 9.079 1.315 42.66 2.218 0.7933 17.17
1 h 8.083 1.718 37.68 2.522 0.8026 7.22
2 h 8.780 1.536 36.40 2.438 0.8068 9.25
4 h 9.179 1.509 38.55 2.313 0.8110 10.79
6 h 8.688 1.413 42.03 2.249 0.8285 19.30
8 h 8.573 1.277 42.56 2.228 0.8176 18.01
24 h 9.050 1.376 42.52 2.208 0.8309 18.38
20–60 °C for 20 times Before 8.820 1.437 42.11 2.181 0.8352 17.64
1 h 9.145 1.807 35.35 2.454 0.8211 11.97
2 h 9.147 1.788 35.16 2.472 0.8145 9.16
4 h 9.431 1.625 37.26 2.415 0.8357 13.89
6 h 9.540 1.606 38.10 2.427 0.8306 12.27
8 h 9.246 1.528 39.47 2.268 0.8469 15.51
24 h 9.224 1.468 42.97 2.175 0.8295 18.50
20–70 °C for 1 time Before 7.404 1.311 42.09 2.208 0.8181 21.41
1 h 7.264 1.978 35.50 2.705 0.8167 3.19
2 h 7.585 1.825 35.83 2.648 0.8034 4.26
4 h 6.932 1.631 36.41 2.406 0.8140 7.71
6 h 7.247 1.560 40.69 2.318 0.8222 16.64
8 h 7.393 1.391 42.24 2.235 0.8258 19.08
24 h 7.270 1.374 41.45 2.233 0.8003 20.71
20–70 °C for 10 times Before 7.222 1.496 40.90 2.137 0.8514 23.64
1 h 6.889 2.137 32.05 2.694 0.7954 3.05
2 h 7.427 2.029 32.61 2.633 0.8023 4.63
4 h 7.435 1.967 33.13 2.574 0.8139 6.49
6 h 7.412 1.986 33.35 2.495 0.8107 9.65
8 h 7.396 1.847 34.00 2.463 0.8065 10.12
24 h 7.539 1.611 39.42 2.559 0.8051 7.13
20–70 °C for 20 times Before 6.563 1.292 39.96 2.111 0.8349 23.93
1 h 6.518 1.957 31.64 2.780 0.8072 1.57
2 h 6.535 1.943 31.00 2.762 0.8088 1.88
4 h 6.776 1.872 34.14 2.617 0.8095 3.70
6 h 6.623 1.896 34.21 2.574 0.7910 5.10
8 h 6.831 1.865 34.58 2.585 0.7876 5.21
24 h 6.607 1.641 37.67 2.500 0.7808 9.27

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Received: 2022-12-30
Accepted: 2023-12-12
Published Online: 2024-03-18
Published in Print: 2024-06-25

© 2024 Walter de Gruyter GmbH, Berlin/Boston

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https://doi.org/10.1515/corrrev-2022-0123
Keywords for this article
repassivation; thermal cycle; passive film; buckling

Articles in the same Issue

  1. Frontmatter
  2. Reviews
  3. Hydrogen in metallic alloys ─ embrittlement and enhanced plasticity: a review
  4. Sacrificial anode materials to protect marine grade steel structures: a review
  5. Original Articles
  6. A new method to estimate the partition of corrosion inhibitors
  7. Corrosion characteristics of in situ hybrid (Al3Ni + Al2O3)/Al composites synthesized by the solid-state combustion
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