# Effects of Temperature on Corrosion Behavior of Reinforcements in Simulated Sea-Sand Concrete Pore Solution

^{1}

^{2}

^{3}

^{4}

^{*}

## Abstract

**:**

_{corr}(corrosion potential) and i

_{corr}(corrosion current density) of the reinforcing steels are temperature and/or chloride concentration (C

_{Cl})-related parameters. A linear correlation between E

_{corr}and temperature and a natural logarithmic correlation between i

_{corr}and C

_{Cl}are observed. It is proved that the relationship between the corrosion rate and temperature follows the Arrhenius equation, whereas the activation energy of corrosion reaction increases with the increase of C

_{Cl}.

## 1. Introduction

_{Cl}) reaches a critical level, the passive film will be broken, and corrosion is initiated [4,5]. Based on Tuutti’s model [10], the corrosion of reinforcements in concrete usually can be divided into two stages: i.e., the initiation and the propagation stages (Figure 1a). However, providing that the chlorides introduced by sea-sands are higher than the threshold value, the corrosion of reinforcement may skip the first initiation stage and go to the second propagation stage immediately after concrete placement. This phenomenon could be called the sea-sand house corrosion model (Figure 1b).

_{corr}(corrosion potential) and i

_{corr}(corrosion current density), were carried out in this study to explore the corrosion behavior of reinforcing steel in a simulated pore solution of sea-sand concrete under different chloride concentrations and temperatures. The relationship between the i

_{corr}of reinforcing steel and temperature was then deduced with the Arrhenius equation. The activation energy of the reinforcing steel corrosion reaction and the pre-exponential factor with different C

_{Cl}were obtained by calculation. A unified equation describing the relationship between the i

_{corr}, temperature and C

_{Cl}was also developed.

## 2. Experimental Program

- (a)
- The samples are immersed in acid solution, containing HCl (HCl: H
_{2}O = 1:1 by volume) and urotropine (3 g/L). - (b)
- After a 2~3 min ultrasonic shower, oxide skins and surface corrosion are cleaned with a brush.
- (c)
- The samples are rinsed with deionized water and are soaked in acetone solution for 2~3 s.
- (d)
- Copper wire is welded at one end of each steel sample after drying.
- (e)
- Both ends of each sample are coated with epoxy resin, leaving a 10 cm length uncoated (a sketch of the coating geometry is shown in Figure 2).

_{2}solution was used as the alkaline electrolyte solution to simulate concrete pore solution, which is thought to be close to the condition in actual pore solution [19,29,30,31,32,33,34]. To simulate a chloride-induced corrosion environment, NaCl was added to the simulated pore solution with concentrations ranging from 0.078~0.727 mol/L. All chemicals used in this experiment were analytical reagents, and distilled water was used as a solvent. To evaluate the influence of temperature on corrosion performance, the immersion solution was controlled in a constant temperature state during the experiment using a temperature-controlled water tank, which controlled the temperature varied in a range of 20~50 °C.

_{corr}and i

_{corr}of reinforcement in the simulated concrete pore solution. The reference electrode was a Leici 232/232-01-type saturated calomel electrode, the counter electrode was a Pt, the working electrode was the tested reinforcing steel, and the electrolyte solution was the simulated concrete pore solution. An example of linear polarization fitting is given in Figure 4. A linear equation, as shown in Equation (1), was used to fit the relationship between potential (y) and current (x).

## 3. Results and Analysis

#### 3.1. Classical Testing Curve for Corrosion Potential and Corrosion Current Density

_{corr}and i

_{corr}as function of immersion duration in the simulated concrete pore solution, which is a saturated Ca(OH)

_{2}solution with and without chloride ions, respectively. It can be seen that the E

_{corr}shifts upward and i

_{corr}decreases with the immersion duration in the saturated pore solution without chlorides. In contrast, once the electrolyte contains chlorides, the E

_{corr}shifts downward and i

_{corr}increases with the immersion duration. The difference in the corrosion potential history between these two cases can be explained by the mixed potential theory. After 48 hours of immersion, the E

_{corr}and i

_{corr}reached a stable state. The purpose of conducting the electrochemical measurements after a period of immersion is to obtain a reliable result without other interferences [36,37,38]. Basically, the measurements should be applied until the OCP values are stabilized enough; e.g., less than 2 [39] or 5 mV [40] within 5 min. In our study, the records of corrosion potential and corrosion current density were performed after 48 hours of immersion. It was found that the variations of OCP values were within 3 mV from 24 to 48 h, which is quite stable in our view and the same as the procedure adopted by Lu et al. [41]. Therefore, the results after 48 hours of immersion presented in this study should be reliable and convincing.

#### 3.2. Corrosion Potential of Reinforcement at Different Temperatures and Chloride Concentrations

_{corr}with the temperature and C

_{Cl}in the simulated pore solution. As seen in Figure 6a, the Cl

^{−}in the simulated pore solution lowered the E

_{corr}of reinforcing steel obviously, to an extent of about 200~300 mV, and an increase of C

_{Cl}also decreased the E

_{corr}. When there was no Cl

^{−}in the simulated pore solution, the value of E

_{corr}of the reinforcing steel was roughly between −236 and –249 mV at the detected temperatures; in comparison, once Cl

^{−}was present, the value was roughly between −405 and –573 mV. Based on the work of Hausmann [42], it can be inferred that the reinforcing steel is in the passivation state in the simulated solution without Cl

^{−}, but in the activation state if the C

_{Cl}equals to or is greater than 0.078 mol/L.

_{corr}and temperature in the simulated pore solution, which is consistent with the tendency represented by the Nernst equation [14]. During the analysis, linear regressions of E

_{corr}as a function of T are carried out in samples immersed by solutions with different C

_{Cl}and the obtained coefficients (slopes and intercepts) are shown in Figure 7.

_{corr}-T relationship in Figure 6b dramatically became negative at the condition of 0.072 mol/L Cl

^{−}and then became relatively constant when C

_{Cl}in the range of 0.167 to 0.727 mol/L. This could be the reason that Cl

^{−}exceeding 0.167 mol/L exerts a significant influence on the behavior of metallic passivation and the anodic dissolution rate; however, Cl

^{−}itself does not directly participate in the anodic oxidation or cathodic reduction reactions. So, the C

_{Cl}has a negligible effect on the linear correlation of E

_{corr}-T for Cl

^{−}> 0.0167 mol/L. Figure 7b shows that the intercept of the E

_{corr}-T relationship, roughly obeying the exponential tendency, became more negative when C

_{Cl}increased, implying severer corrosion at the higher temperature.

_{corr}and T, an empirical equation for the estimation of E

_{corr}and T can be established irrespective of whether the reinforcing steel is in the activation or passivation state, as shown in Equation (2), which is valid within the temperature range of 20–50 °C.

_{Cl}). Providing the corrosion potential of steel reinforcement at a certain temperature is known, the E

_{corr}at other temperatures can be estimated based on Equation (2). Using ${T}_{0}$ = 20 °C as the reference temperature, a comparison between the measured and estimated values of the E

_{corr}at different temperatures is illustrated in Figure 6b. All the relative errors between the measured and estimated values are less than 5%.

#### 3.3. Corrosion Current Density of Reinforcements at Different Temperatures and Chloride Concentrations

_{corr}with the C

_{Cl}at different temperatures. It can be seen that the C

_{Cl}has an obvious impact on the i

_{corr}and a higher C

_{Cl}resulting in a larger i

_{corr}. With the increase of the C

_{Cl}from 0.078 to 0.727 mol/L, the i

_{corr}at different temperatures increases by more than double on average, which is a similar trend to that reported by peer researchers. Jiang et al. [43] and Yu et al. [44] proved that C

_{Cl}has a limited effect on i

_{corr}for reinforcing steel with a protective passive film, whereas significant effects were only found for reinforcing steel in the active state. The associations between i

_{corr}and C

_{Cl}may be related to the dissolution rate of the passive film [45] or the adsorption characteristics of Cl

^{−}at the surface of reinforcing steel [46]. Moreover, as chloride ions are mainly in the anodic region, their effects on the anodic reaction are significant, which in turn influences the corrosion current [47].

_{corr}and ${C}_{Cl}$, as seen in Figure 8b. The corresponding equation can be expressed as Equation (3):

_{corr}and ln${C}_{Cl}$ was also reported by Abd El Aal et al. [45], who used simulated pore solution containing chlorides together with Ca(OH)

_{2}. Figure 9 provides regression coefficients of ${a}_{Cl}$ and ${b}_{Cl}$. It is obvious that both coefficients of ${a}_{Cl}$ and ${b}_{Cl}$ are temperature dependent and exponentially increased and decreased, respectively, with the increasing temperatures. Based on the theory of reaction kinetics, the electrode reaction speed (v) is linearly associated with the concentration of the electrode reactant ($c$), while according to Equation (3) obtained from experimental results, i

_{corr}is natural logarithmically related to the C

_{Cl}. Therefore, it can be deduced that Cl

^{−}is not a reactant of the anode electrode reaction of metal anode dissolution; instead, it works as a catalyst for the corrosion reaction.

_{corr}and the current density ratio (i

_{corr},

_{T}/i

_{corr},

_{20}). With an increase in temperature, the polarization resistance of reinforcing steel falls significantly, and the i

_{corr}shows a clear increase. When the reinforcing steel is in the passivation state—i.e., without influence from Cl

^{−}, an increase of 10 °C could lead to a further increase in i

_{corr}by a factor of 1.3~1.8. This illustrates that temperature also has a significant influence on the corrosion rate of reinforcing steel in the passivation state, which is consistent with the studies of Michel et al. [17]. In contrast, once the reinforcing steel is in the activated state, influenced by 0.078~0.727 mol/L of Cl

^{−}, an increase of 10 °C could lead to a 1.4~1.9 times increase in i

_{corr}. Therefore, the effect of temperature on the corrosion rate of reinforcing steel, in either passivated or activated state, makes limited difference, and the values are lower than the previous values from 2 to 4 times, as deduced according to Van’t Hoff’s rule [48].

^{−1}·dm

^{3}·s

^{−1})$,\text{}{E}_{a}$ is the activation energy (kJ·mol

^{−1}), and R is the gas constant. For the electrode system of reinforcing steel corrosion, the value of $k$ cannot be easily and directly measured. Instead, its mathematical relationship with i

_{corr}can be derived from the Stern–Geary equation and Faraday’s law, following the calculation as mentioned in Equations (4)–(9) listed below.

_{corr}and polarization resistance R

_{P}is expressed as Equation (5) [51,52]:

_{corr}of the electrode reaction from metal anode dissolution and the electrode reaction rate can be calculated following Equation (6).

^{3}). Substituting Equation (7) into Equation (6) yields

_{corr}of the reinforcing steel. Substituting Equation (4) into Equation (8), the correlation equation between i

_{corr}and temperature can be obtained as shown in Equation (9).

_{a}/R) is constant for each analysis, which means that the E

_{a}is a temperature-independent factor for the corrosion of reinforcing steel.

^{−1}) and ln(A) (mol

^{−1}·dm

^{3}·s

^{−1}) of the corrosion reaction of reinforcing steel in the simulated pore solutions with various C

_{Cl}are shown in Figure 12. It can be known that E

_{a}decreases with increases in C

_{Cl}, providing the existence of Cl

^{−}, and ranges from 35.8 and 41.5 kJ/mol, which is very close to the values of 35~40 kJ/mol, as presented by Michel et al. [17]. By discarding the value at 0 mol/L Cl

^{−}, the relationship between ${E}_{a}$ and chloride concentration seems unclear, as the value in 0.727 mol/L Cl

^{−}has exceeded the 95% confidence interval. Further study is needed to study this relationship in wider ranges of chloride concentration. Regarding the ln(A), all of the fitted results with the existence of Cl

^{−}are within the 95% confidence interval, which means that ln(A) could be seen as a constant in this condition.

_{a}, or the “−E

_{a}/R”, reveals the sensitivity of the electrode reaction rate to the change in temperature. It can be assumed that the samples immersed in a higher concentration of chloride solution have a lower value of E

_{a}and a corresponding lower temperature sensitivity. This is consistent with the results shown in Figure 10b: for the tests containing Cl

^{−}, the highest increase rate of i

_{corr}due to a change in temperature is in the sample with the lowest C

_{Cl}(0.078 mol/L), for which the E

_{a}is the highest.

_{Cl}and T, as described in Equations (2) and (9), a unified equation for the three variables can be deduced as the Equation (11):

_{Cl}, T and $\mathrm{ln}{i}_{corr}$, the values of ${a}_{T,Cl}$,${b}_{T,Cl}$ and ${c}_{T,Cl}$ are obtained, which have the values of 18.4, 0.39 and −4691, respectively, and the coefficient of fitting R

^{2}is about 0.99. Therefore, the corrosion current density of the reinforcing steel in the simulated pore solution that has a chloride concentration and temperature can be determined based on the empirical relationship as shown in Equation (12).

## 4. Conclusions

_{corr}and temperature. The slope of the linear correlation is related only to the corrosion state of the reinforcing steel—i.e., the passivation or activation—and this slope is independent of the chloride concentration C

_{Cl}in the simulated pore solution.

_{corr}. When the chloride concentration increases from 0.078 to 0.727 mol/L, i

_{corr}values at different temperatures are more than doubled on average. There is a natural logarithmic correlation between i

_{corr}and chloride concentration in the simulated pore solution.

_{corr}. The relationship between corrosion rate and temperature T is found to be well described by an Arrhenius equation within the experimental temperature range. The activation energy E

_{a}of the corrosion reaction decreases with increasing chloride concentration in the simulated pore solution. However, there is no clear correlation between the pre-exponential factor A and chloride concentration.

## Author Contributions

## Funding

## Data Availability Statement

## Acknowledgments

## Conflicts of Interest

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**Figure 1.**Schematic sketch of steel corrosion model in concrete: (

**a**) Tuutti model [10]; (

**b**) sea-sand house model.

**Figure 5.**Developments of E

_{corr}(

**a**) and i

_{corr}(

**b**) during immersion in simulated concrete solution.

**Figure 8.**Relationship between current density and chloride concentration: (

**a**) i

_{corr}vs. C

_{Cl}; (

**b**) lni

_{corr}vs. lnC

_{Cl}.

**Figure 9.**Regression coefficients of lni

_{corr}-lnC

_{Cl}relationship: (

**a**) ${a}_{Cl}$; (

**b**) ${b}_{Cl}$.

**Figure 10.**Relationship between current density and temperature: (

**a**) i

_{corr}vs. temperature; (

**b**) ratio of i

_{corr},

_{T}/i

_{corr},

_{20}vs. temperature.

Fe | C | Mn | Si | P | S |
---|---|---|---|---|---|

98.96 | 0.21 | 0.63 | 0.17 | 0.005 | 0.026 |

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**MDPI and ACS Style**

Xia, S.; Luo, Y.; Li, Y.; Liu, W.; Ding, X.; Tang, L.
Effects of Temperature on Corrosion Behavior of Reinforcements in Simulated Sea-Sand Concrete Pore Solution. *Buildings* **2022**, *12*, 407.
https://doi.org/10.3390/buildings12040407

**AMA Style**

Xia S, Luo Y, Li Y, Liu W, Ding X, Tang L.
Effects of Temperature on Corrosion Behavior of Reinforcements in Simulated Sea-Sand Concrete Pore Solution. *Buildings*. 2022; 12(4):407.
https://doi.org/10.3390/buildings12040407

**Chicago/Turabian Style**

Xia, Song, Yaoming Luo, Yongqiang Li, Wei Liu, Xiaobo Ding, and Luping Tang.
2022. "Effects of Temperature on Corrosion Behavior of Reinforcements in Simulated Sea-Sand Concrete Pore Solution" *Buildings* 12, no. 4: 407.
https://doi.org/10.3390/buildings12040407