Anticorrosion properties of ionic liquid functionalized graphene oxide epoxy composite coating on the carbon steel for CCUS environment

doi:10.21203/rs.3.rs-5241126/v1

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Anticorrosion properties of ionic liquid functionalized graphene oxide epoxy composite coating on the carbon steel for CCUS environment

https://doi.org/10.21203/rs.3.rs-5241126/v1

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The adoption of CO₂ capture, utilization, and storage (CCUS) technology is increasingly prevalent, driven by the global initiative to conserve energy and reduce emissions. Nevertheless, CCUS has the potential to induce corrosion in equipment, particularly in high-pressure environments containing CO₂. Therefore, anti-corrosion protection is necessary for the metal utilized for CO₂ production and storage equipment. Herein, an ionic liquid (Triethylsulfonium bis-trifluoromethylsulfonyl-imide) was used to functionalize graphene oxide (prepared via improved Hummers method). FESEM, TEM, and XPS confirmed ionic liquids (IL) were successfully attached to the GO lattice. Afterwards, 0.5 wt% and 1 wt% IL-GO composites were separately incorporated into the epoxy and coated on the carbon steel substrate with a thickness of 50 ± 2 µm. The surface examinations demonstrated a consistent distribution of the ILGO composite in the epoxy matrix and achieved a uniform surface. Anti-corrosive property of 0.5 wt% and 1 wt% IL-GO/epoxy coatings was evaluated using electrochemical tests such as potentiodynamic polarisation, and electrochemical impedance spectroscopy (EIS) after immersion in the CO₂ (1.5 MPa) and 3.5 wt% NaCl system. After 48 h of immersion in a corrosion environment (CO₂-NaCl), the protection efficiency of 0.5 wt% and 1 wt% IL-GO/epoxy coatings are 86.41 ± 0.55 and 92.59 ± 0.83%, respectively. The findings of this study demonstrated that the ILGO composite reinforced epoxy coating exhibited exceptional corrosion resistance when exposed to CO₂.

carbon steel

ionic liquid

graphene oxide

CO2

epoxy coating

electrochemical studies

With the increase in worldwide temperature, the melting ice is leading to an increase in sea level (Yuan et al. 2022a; Velpandian et al. 2023; Dhongde et al. 2024b). Consequently, an increasing number of countries are prioritizing the reduction of carbon dioxide (CO₂) emissions in industrial sectors (Feng et al. 2023). During the CCUS process, it is unavoidable for compressed solutions containing CO₂ gas and other organic/inorganic ions to come into contact with transportation pipelines and metal reaction equipment (Wang et al. 2024b). Hence, the issue of metal equipment corrosion resulting from the CCUS process must not be overlooked.

Carbon steels are widely used in various industrial applications, including the CCUS technology, gas storage wells, production systems for oil and gas industries, and ship construction (Sun et al. 2023a; Devi et al. 2024; Adhikari et al. 2024). They are affordable and offer numerous benefits in terms of mechanical, electrical, and thermal properties (Talukdar and Rajaraman 2020; Talukdar et al. 2022, 2023). They potentially experience severe corrosion when chlorine compounds and corrosive gases (H₂S, CO₂, etc.) are available in the production well (Zhou et al. 2024; Yin et al. 2024a). Among various anti-corrosion measures such as cathodic protection, corrosion inhibition, corrosion-resistant alloys, and anti-corrosion coating, anti-corrosion coating are more reliable and cost-effective techniques for carbon steel protection in the corrosive environment (CO₂ and NaCl) (Sun et al. 2023b; Yin et al. 2024a).

An epoxy-based coating is the most favourable for carbon steel protection in corrosive environment (Henriques and Soares 2024). The epoxy resins are highly compressible substances with exceptional resistance to corrosion, high tensile strength, durability against physical damage, and superior fatigue resistance (Diraki and Omanovic 2023; Cui et al. 2023). However, the service life of the epoxy-based coating is limed. Furthermore, to enhance the resistance to corrosion and prolong the lifespan of the epoxy-based coating, multiple fillers were employed (Balakrishnan et al. 2024; Dhongde et al. 2024a). Hence, numerous modified fillers were used in the epoxy coating to increase the lifespan and anti-corrosive property (Sasidharan and Anand 2020; Diraki and Omanovic 2022).

There are various types of fillers, including polymer-based, lubricant fillers, carbon-based, metallic, ceramic, and mineral silicates. In recent years, researchers are working on modified carbon-based fillers(Randis et al. 2023) and graphene oxide (GO) is one of the most popular fillers for the epoxy coating (Oliveira et al. 2023). The phenomenon of graphene oxidation has garnered significant attention in recent times, primarily driven by the potential utilization of GO as a means to achieve cost-effective synthesis of substantial quantities of graphene (Ashok Kumar et al. 2023). Moreover, the majority of studies have focused on the conventional Hummers' method for synthesizing GO due to its high efficiency and satisfactory safety during the reaction (Yu et al. 2016). Nevertheless, the oxidation process utilized in these preparation methods results in the emission of hazardous gases like NO₂ and N₂O₄, which presents an added difficulty in eliminating the residual $\:{Na}^{+}$ and $\:{NO}_{3}^{-}$ ions from the waste generated during the GO production procedures (Chen et al. 2013; Dhongde et al. 2023a; Patil et al. 2024; AlHumaidan et al. 2024). In this study, the improved Hummers' method was chosen instead of the conventional Hummer's method for synthesizing GO. The improved method, developed by Marcano et al. (Marcano et al. 2010), is more environmentally friendly as it eliminates the use of NaNO₃, increases the amount of KMnO₄, and involves a reaction with H₂SO₄ and H₃PO₄ in a 9:1 ratio (by volume). This improvement effectively increased the reaction yield and easily reduced the generation of harmful gases by controlling the reaction temperature. Nevertheless, the potential uses of GO are limited due to its inadequate ability to disperse in epoxy matrices and solvents. Over the years, several techniques have been devised to enhance the ability of GO to disperse and to improve its compatibility with polymers.

Ionic liquids (IL) are considered to be highly favorable options for a wide range of applications, including corrosion inhibition, supercapacitors, and electrochemical devices (Dutta et al. 2022, 2024; Dhongde et al. 2023c). Researchers have shown great interest in synthesizing nanomaterials that are functionalized with IL due to their remarkable solubility, lack of volatility, and environmentally advantageous properties (Yu et al. 2016; Lavin-Lopez et al. 2016). Functionalized GO has been extensively studied in academic, government, and commercial research settings (Chen et al. 2013). Chengbao et al (Liu et al. 2018a), examined the IL (amino-terminated) modified with GO/epoxy coating for the corrosive protection application in 3.5 wt% NaCl. Y Wu et al. (Wu et al. 2020), prepared fluorinated reduced GO via modified Hummer’s method and then modified with acrizidinium IL for corrosive protection application in 3.5 wt% NaCl. Dhongde et al. (Dhongde et al. 2023b), employed the alkyl imidazolium IL for the modification of GO (improved Hummer’s method) and used for the anticorrosive application in 3.5 wt% NaCl. However, the utilization of IL modified GO composite (ILGO) as fillers for epoxy coating in CCUS applications remains unexplored.

Only few works were reported for anti-corrosive applications of epoxy-based coating for CCUS. Qianqian Yin et al(Yin et al. 2024a) prepared poly (α-cyanoethyl acrylate) on mica filler for epoxy coating and anticorrosion performance was measured after immersion in the CO₂ (Pressure: 1.5 MPa). Yue Sun et al (Sun et al. 2023b). synthesized g-C₃N₄ (Graphitic carbon nitride) and epoxy silane oligomer to shield carbon steel from CO₂ (Pressure: 3.0 MPa) in CCUS technology. Yue Sun et al (Sun et al. 2024a). have successfully grown C₃N₄ (Nanosheet) and CeO₂ (Nanorod) on the surface of a micron sheet basalt). This coating was used in CCUS technology to protect metal surfaces. Thus, to the best of the author’s knowledge, ionic liquids have not been explored as a filler in epoxy coating for the protection of carbon steel in CCUS applications till now.

In this work. specifically, triethylsulfonium bis-trifluoromethylsulfonyl-imide IL which have relatively low melting point and low viscosity has been considered as a filler. Tomoko Sugizaki et al. (Sugizaki et al. 2023). used triethylsulfonium bis-trifluoromethylsulfonyl-imide IL in electrolytes for Li metal batteries (Li-ion batteries application) and reported IL have relatively low melting point and low viscosity. Therefore, the primary objective of the present work is to analyses the corrosion protection behavior of the ILGO filler in epoxy coating after immersion in CO₂-NaCl medium.

2.1 Materials

Graphite powder (particle size ≥ 100 mesh), Triethylsulfonium bis-trifluoromethylsulfonyl-imide, 4–4’-diaminodiphenyl sulfone (DDS), and bisphenol A diglycidyl ether (BADE) were obtained from Sigma-Aldrich. Additional chemical reagents such as sodium chloride (NaCl), potassium permanganate (KMnO₄), hydrogen peroxide (H₂O₂), potassium hydroxide (KOH), sodium hydroxide (NaOH), hydrochloric acid (35%), ortho-phosphoric acid (88%), and sulfuric acid (98%) used in this work are all of analytical grade. The carbon steel metal (Fabricated from Aries Engineers Pvt. Ltd., Maharashtra, India) was used as a coating substrate with the dimension of 13 × 3 mm. The chemical compositions of the carbon steel are presented in Table 1.

Table 1

Chemical composition (wt.%) of the carbon steel.
Element	Ti	S	V	P	Si	Mn	Nb	V	C	Fe
Wt.%	0.005	0.007	0.004	0.009	0.23	0.82	0.003	0.004	0.13	Bal.

2.2 Synthesis of GO via improved Hummer’s method

90 ml of sulfuric acid (H₂SO₄) and 10 ml of ortho-phosphoric acid (H₃PO₄) were combined in a ratio of 9:1. The mixture was rigorously mixed in a round bottom flask using a magnetic stirrer (Tarsons Products Limited, India) for 20 min at a speed of 800 rpm. The H₂SO₄ served as an intercalator in the graphite, while H₃PO₄ was employed to augment the intercalation process. Subsequently, a cumulative quantity of graphite (2 gm) was incrementally added to the agitating mixture, in minute portions. After stirring the solution for an additional 15 min, 6 gm. of KMnO₄ were added and agitated for approximately 1 hr. During this phase, the temperature was consistently kept within the range of 1–4°C. Afterward, the mixture was thoroughly mixed for a period of 12 hr. at 25 ± 2°C. Afterward, 100 mL of DI water were added incrementally, with one drop being added at a time. Ultimately, the process of oxidation was stopped by introducing 20 mL of hydrogen peroxide (30%). The GO was synthesised by centrifuging the suspension, then washing with HCl (1 M) and DI water several times. The GO was then dehydrated in a vacuum oven at a temperature below 60 ± 2°C until it converted into powdered GO.

2.3 Preparation of ILGO

The uniform distribution was achieved by dissolving 1 gm of GO in DI water using ultrasonication for a duration of 1 hr. 0.2 gm of IL and 0.5 gm of KOH were added to the solution, which was then subjected to ultrasonic processing for a duration of 60 min. The uniform solution was vigorously stirred at a temperature of 90 ± 2 ⁰C for a duration of 36 hr to produce the ILGO composite. After undergoing multiple centrifugation cycles with deionized water and ethanol, the resulting ILGO solution was subsequently dried in a vacuum oven at temperatures below 60 ± 2°C. The ILGO composite was stored at a temperature range of 2–6°C.

2.4 ILGO coatings on carbon steel substrate

The mixture consists of 1.25 mg of ILGO and 150 mg of hardener. It is combined with 10 mL of DI water and stirred on a magnetic stirrer for 30 min at room temperature. After that, it is sonicated for 90 min. Subsequently, 100 mg of epoxy was introduced into sonicated mixture to create a 0.5 wt% ILGO/epoxy solution. The resulting solution was then subjected to magnetic stirring for a duration of 2 hr. to ensure thorough blending. To prevent the occurrence of defects during the coating procedure, the epoxy was subjected to a 30 min vacuum-drying process in an oven. The carbon steel substrate underwent grinding with silicon carbide (SiC) sheets of increasing grades (180, 320, 600, and 1000), followed by polishing via alumina powder (1.0 µm and 0.3 µm). Following the cleaning of carbon steel with DI water, any particles that had attached to the substrate were removed using ultrasonication. Lastly, employing compressed air any remaining moisture was eliminated. A carbon steel substrate was then coated with a precise thickness of 50 ± 3 µm using a four-sided thin film applicator. Ultimately, a duration of 5 days was allocated for the process of curing. The carbon steel was coated with 0.5 wt% ILGO/epoxy using the same method.

2.5 Characterization

The surface morphology of GO and ILGO was studied using a field emission scanning electron microscope (FESEM, Zesis, Sigma 300) and high-resolution transmission electron microscope (FETEM, JEOL 2100). The chemical composition of GO and ILGO was determined through X-ray photoelectron spectroscopy (XPS) (PHI5000VersaProbe III, ULVAC-PHI, INC) employing monochromatic Al K-α source at a take-off angle of 45⁰. The XPS spectra were obtained utilizing the SmartSoft-XPS v2.0 (PHI) software. The water contact angle was measured utilizing a goniometer (Holmarc Opto-Mechatronics, model: HO-IAD-CAM-01B) with a DI water droplet volume of 3 µL at the ambient temperature (28 ± 2 ⁰C) and a relative humidity of 65 ± 2%.

2.6 Corrosion tests

Initially, the coated carbon steel sample was inserted in the Parr Autoclave reactor. The coating samples were exposed to the corrosive environment of CO₂ (1.5 MPa) at a temperature of 30 ℃ and 3.5 wt.% NaCl (300 ml). Following a 48 hr treatment in the Parr Autoclave reactor, the coated carbon steel sample was cleaned with DI water to eliminate any corrosive substances or residue from the coating's surface.

Electrochemical activity of coated sample exposed to CO₂ environment has measured using an electrochemical workstation (Gamry Interface 1010E). For all electrochemical tests, a 300 mL fresh solution of 3.5 wt% NaCl was used as an electrolyte. A three-electrode system has employed for the electrochemical measurements and consists of a working electrode (coated carbon steel electrode with an exposed area of 0.78 cm²), a counter electrode (platinum wire), and a reference electrode (Ag/AgCl 3 M KCl). Electrochemical measurements were conducted exclusively once the open circuit potential (OCP) had attained a stable value. The potentiodynamic polarisation analysis were carried out from − 250 to 250 mV w.r.t OCP at a scan rate of 1 mV/s. At OCP, the electrochemical impedance spectroscopy (EIS) analysis with a frequency range of 10 kHz to 10 mHz and a sinusoidal perturbation of ± 10 mV amplitude were performed. The ZSimpWin software was used to fit the EIS data using an electrical equivalent circuit (EEC) model.

3.1 Morphology of GO and ILGO:

The morphology of GO and ILGO were presented in FESEM (Fig. 1). The lamellar structure is evident in both GO and ILGO. In particular, the FESEM image of ILGO (Fig. 1b) reveals the connection of multiple monolayers to form larger sheets. The presence of small lamellae in the ILGO (Marked inside Fig. 1b) indicates that the GO lamellae have been fragmented into multiple distinct layers as a result of the van der Waals interaction (Liu et al. 2018a; Shen et al. 2021). The FESEM result demonstrated that the modification of GO by IL was effective.

The TEM image of GO and ILGO were presented in the Fig. 2(a and b). In the TEM picture of GO (Fig. 2a), the sheet that was seen was unfortunately made up of several layers. After the modification with IL, thin layer structure and translucent is observed, which a clear evidence from the successful modification of GO sheet with IL. Finally, the HRTEM image with the lattice fringes were presented in the Fig. 2c.

3.2 X-ray photoelectron spectroscopy (XPS) analysis:

The surface composition of the ILGO was analysed by XPS. Figure 3 gives the high-resolution C 1s spectra of the GO and ILGO. The C1s spectrum of GO shows carbon bonds at 284.6 eV, 286.7 eV, and 287.8 eV, resulting from the C = C (sp² bonded carbons), C-O (epoxy/hydroxyls), C = O (carbonyl), respectively. This outcome provides additional validation that they possess similar levels of oxidation. It is important to mention that the oxidation levels of GO products differ depending on the conditions under which they are synthesized. The results from FESEM, TEM, and XPS confirmed the successful synthesis of GO using an improved Hummers method, resulting in a higher level of purity. The C1s spectra of ILGO shows four carbon components at 284.7 eV (C-C), 285.2 eV (C-N), 286.8 eV (C-O), and 288.1 eV (N-C = O) (Liu et al. 2018a; Dhongde et al. 2023b). More precisely, the presence of the N-C = O bond, indicates that amide bonds were formed between the amino group of IL and the carboxylic acid groups of GO. The existence of a C-N bond demonstrates the attachment of an IL to GO nanosheets through a ring opening reaction (Liu et al. 2018a; Dhongde et al. 2023b).

3.3 Characterization of coating:

3.3.1 Morphology analysis by FESEM measurements:

The cross-sectional morphology of epoxy, 0.5 wt% ILGO/epoxy, and 1 wt% ILGO/epoxy coatings was characterized using FESEM after 48 hr treatment in the CO₂-NaCl. As depicted in Fig. 4a, the epoxy coating shows the ununiform and brittle fractures surface. Fig. S1 (Supplementary File) displays the FESEM image of the 1 wt% GO/epoxy coating subsequent to treatment with a CO₂-NaCl medium. The aggregation of the GO in the epoxy resulted in an uneven surface. The existence of holes and pores in the epoxy and 1 wt% GO/epoxy coatings indicates that the corrosive solution (CO₂-NaCl) has infiltrated the barrier coating and engages with the carbon steel. Upon incorporating 0.5 and 1 wt% ILGO into the epoxy, no holes or pores were detected on the surface, leading to a more compact surface, as depicted in Fig. 4b-c. The even distribution of ILGO within the epoxy resulted in a sleek surface and improved the coating's density. This suggests that the interfacial interaction between ILGO and epoxy is more robust (Wu et al. 2020; Cheng et al. 2021). Additionally, ILGO enhanced the relationship between the hardener and epoxy. The results of the FESEM analysis indicated that the superior dispersion characteristics of the ILGO composite could improve the anticorrosion properties of coatings.

3.3.4 Contact angle measurement:

Figure 5 displays the results of the water contact angle measurements on the prepared coatings. The water contact angle of various coating was recorded after 48 hr treatment in CO₂-NaCl medium. The lowest water contact angle was recorded for the pure epoxy (60.68⁰). The water contact angle for 0.5 and 1 wt% ILGO/epoxy, coating was 67.91⁰ and 75.31⁰ observed. Due to the addition of 0.5 and 1 wt% ILGO in the epoxy contact angle values increase but not significantly. The water contact angle results suggest that the surface exhibits water repellent characteristics (Ziat et al. 2020; Sun et al. 2022).

3.4 Corrosion test of the coating:

3.4.1 Potentiodynamic polarisation test

A potentiodynamic polarisation analysis was employed to assess the anti-corrosion performance of epoxy, 0.5 wt% ILGO/epoxy, and 1wt% ILGO/epoxy coating after 48 hr, of treatment with CO₂-NaCl medium. Fresh 3.5 wt% NaCl solution was used as an electrolyte solution (300 mL) for the potentiodynamic polarisation test. The results obtained from potentiodynamic polarisation analysis are presented in Fig. 6. A significant drop in the anodic current density and anodic current density is observed for the coated substrates in the order epoxy < 0.5 wt% ILGO/epoxy < 1 wt% ILGO/epoxy. The presence of 0.5 wt% ILGO/epoxy and 1 wt% ILGO/epoxy coating significantly slow down the rates at which oxygen is reduced (cathodic reaction) and carbon steel dissolves (anodic reaction). The values of corrosion potential (E_corr), corrosion current density (i_corr), anodic Tafel slope (β_a), and cathodic Tafel slope (β_c) obtained from these plots are documented in Table 2. Additionally, the polarisation resistance (R_p) and protection efficiency (PE) were calculated using the Stern-Geary equation provided below (Li et al. 2022; Kumar and Das 2023, 2024; Farhat et al. 2024):

$$\:{R}_{p}\left(\text{k}{\Omega\:}\:{\text{c}\text{m}}^{2}\right)=\frac{{\beta\:}_{a}{\beta\:}_{c\:\:}}{{{2.303(\beta\:}_{a}+{\beta\:}_{c\:\:})i}_{corr}}$$

$$\:\text{P}\text{E}\left(\text{\%}\right)=\frac{{i}_{corr,o}-{i}_{corr,i}}{{i}_{corr.o}}\times\:100$$

Where i_corr,o and i_corr,i denote the corrosion current density (A/cm²) of the without and with coated carbon steel substrate, respectively.

Table 2

Electrochemical parameters obtained from the polarization curves
Sample	-E_corr (V) versus Ag/AgCl	i _corr (µA/cm²)	βa (V/dec)	-βc (V/dec)	R_p (kΩ cm²)	PE (%)
Epoxy	0.71 ± 0.024	0.81 ± 0.010	0.63 ± 0.014	0.49 ± 0.016	62.40 ± 0.15	-
0.5wt% ILGO/epoxy	0.65 ± 0.018	0.11 ± 0.008	0.92 ± 0.014	0.69 ± 0.021	1088 ± 19.21	86.41 ± 0.55
1wt% ILGO/epoxy	0.59 ± 0.196	0.06 ± 0.00	0.48 ± 0.020	0.27 ± 0.016	2817.05 ± 28.22	92.59 ± 0.83

The lower value for i_corr (0.06 µA/cm²) and higher value for E_corr (-0.59 V) for the 1 wt% ILGO/epoxy coating suggest the corrosion-inhibiting performance was better against the CO₂. The PE (%) for 0.5 and 1 wt% ILGO/epoxy coating was measured to be 86.41 ± 0.55 and 92.59 ± 0.83 (%), respectively. Typically, a higher R_p value indicates a higher level of anticorrosive properties in the coating. The highest R_p value (2817.05 kΩ cm²) was noted for the 1wt% ILGO/epoxy coating. This suggests that the addition of just 1wt% ILGO significantly improves the anti-corrosion properties of epoxy coating in corrosive environments. However, the lowest R_p value (62.40 kΩ cm²) was observed for the epoxy coating. When coating is subjected to pressure, a portion of the CO₂ molecules in the solution undergoes a reaction with water molecules, resulting in the formation of ionizable carbonic acid (El-Fattah et al. 2024; Wang et al. 2024c; Yin et al. 2024a). This reaction also leads to the production of mixed corrosion species in the solution. While the curing process of pure epoxy coating occurs, the formation of small voids inside the coating occurs as a result of the alteration of internal and external stresses. CO₂ molecules infiltrate the surface of the carbon steel substrate alongside carbonic acid molecules within the coating, propelled by pressure (Sun et al. 2023b; Zargarnezhad et al. 2023; Fan et al. 2024). The carbonic acid molecules undergo a chemical reaction with the steel substrate as a result of significant polarization, leading to carbon steel corrosion (Sun et al. 2023a, b; Zhou et al. 2024). The 0.5 and 1 wt% ILGO/epoxy coating does not exhibit any visible pores or flakes in the coating, as shown in Fig. 1. This lack of pores and flakes hinders the absorption of CO₂ gas and the prevention of chloride ions, H₂O, and other corrosive solutions from penetrating the coating. When compared to epoxy coating, both the concentrations of ILGO (0.5 wt% and 1 wt%) demonstrate higher levels of protection efficiency. This suggests that the ILGO are evenly distributed throughout the epoxy matrix without any noticeable clumping. The experiment was also conducted using a 1.5 wt% ILGO /epoxy mixture. Nevertheless, the decline in potential energy was detected as a result of the accumulation of ILGO in the epoxy matrix.

3.4.2 EIS measurements:

The EIS test was used to measure the anticorrosion properties of ILGO/epoxy coating. Figures 7 and 8 show the Nyquist and Bode plots of the epoxy, 0.5 wt% ILGO/epoxy, and 1 wt% ILGO/epoxy coating in the NaCl solution (3.5 wt%). The solid continuous curve in Fig. 7 denotes the results of fitting the EIS data with the electrical equivalent circuit. The experimental findings that were recorded are represented by the dotted curve in Fig. 7. The Nyquist diagram (Fig. 7) of the coatings, following a 48-hour treatment in a CO₂-NaCl corrosion environment, exhibited a significant semicircular capacitive arc, which suggests a high level of effectiveness in preventing corrosion. The low-frequency impedance modulus (|Z|_{0.01 Hz}) can serve as an indicator for assessing the corrosion resistance of different coatings (Wang et al. 2024a; Zargarnezhad et al. 2024). After 48 hr of immersion in a CO₂-NaCl corrosion environment, the |Z|_{0.01 Hz} values of pure epoxy, 0.5 wt% ILGO/epoxy, and 1 wt% ILGO/epoxy coatings were 4.91 $\:\times\:$ 10³, 2.45 $\:\times\:$10⁶, and 4.03 $\:\times\:$ 10⁶ (Ω cm²) respectively. The |Z|_{0.01 Hz} value for the coatings containing 0.5 wt% and 1 wt% of ILGO in an epoxy matrix was increased compared to the coatings without ILGO. The ILGO filler enhanced the reinforcement and compactness of the epoxy matrix, resulting in an increased anticorrosion property of the coating. Ultimately, the even and consistent distribution of the ILGO fillers within the epoxy matrix effectively hindered the penetration of CO₂-NaCl and water into the coating. Prolonged exposure to a corrosive solution (CO₂-NaCl) induces alterations associated with the carbonation of ILGO composite within the epoxy matrix and the formation of micropores (Zargarnezhad et al. 2024). These modifications encompass the fluctuation in Z’ and |Z|_{0.01 Hz}., as depicted in Fig. 8. The Bode plot (Fig. 8) clearly demonstrates the superior anticorrosion performance of 0.5 wt% and 1 wt% ILGO/epoxy coatings compared to epoxy coating.

The EEC modelling technique was employed to quantitatively evaluate the anticorrosion properties of epoxy, 0.5 wt% ILGO/epoxy, and 1 wt% ILGO/epoxy coating. The EEC parameters were estimated using the ZSimpWin software. The chosen comparable circuit (Fig. 9) exhibits a high level of accuracy, as indicated by its best fit quality (χ² < 0.01). The variables R_s, Q_c, R_pore, Q_dl, and R_ct in the model correspond to the solution resistance, capacitance, pore resistance, double layer capacitance, and charge transfer resistance, respectively. The development of pores in the outer layer (denoted by R_s and Q_c) and the elevated impedance of the intact inner layer (indicated by R_ct and Q_dl) can be discerned through an Equivalent Electrical Circuit (EEC) to analyze the system's behavior (Fig. 9). This representation remains valid until a significant coating failure occurs (Trentin et al. 2022; Zargarnezhad et al. 2024). The similar EEC circuit with Qc and Qdl was also used in previous studies (Wang et al. 2020; Yuan et al. 2022b; Sun et al. 2024b). Instead of using an ideal capacitor, it is suggested to use a constant-phase element (CPE, Q) to achieve more accurate fitting outcomes. The given equation represents the impedance of CPE.

$$\:Z=\frac{{\left(j\omega\:\right)}^{-n}}{{Y}_{0}}$$

$$\:Q={Y}_{0}({{\omega\:}_{max})}^{n-1}$$

The ω_max represents the angular frequency, Y₀ represents the CPE parameter, and j represents the imaginary root. The ω_max represents the frequency that is linked to the highest Z_imag value. When the value of n is 1, the CPE is corresponding to an ideal capacitor, whereas when n is 0, it represents a resistor. The value of n varies from 1 as a result of the heterogeneities present on the electrode surface(Cheng et al. 2021; Dhongde et al. 2024a). Figure 10(a-b) shows the obtained significant EEC values. Reduced values of Q_c and Q_dl point to lower porosity and improve resistance to corrosive fluid intrusion. In Fig. 10(a), the values of Q_c and Q_dl for 0.5 wt% ILGO/epoxy (4.81×10^− 11 Fcm^− 2Sⁿ⁻¹ and 8.01×10^− 12 Fcm^− 2Sⁿ⁻¹) and 1 wt% ILGO/epoxy (5.47×10^− 11 Fcm^− 2Sⁿ⁻¹ and 9.10×10^− 12 Fcm^− 2Sⁿ⁻¹) were very low compared to pure epoxy (4.61×10^− 7 Fcm^− 2Sⁿ⁻¹ and 3.21×10^− 7 Fcm^− 2Sⁿ⁻¹). In previous studies (Liu et al. 2018b; Ye et al. 2021; Zhou et al. 2022; Henriques et al. 2024), similar trends of Qc and Qdl were observed. In general, R_pore is important for the evaluation of film/coating compactness, and R_ct represents the anticorrosion performance of the carbon steel substrate (Liu et al. 2018a). Therefore, the R_pore/ R_ct values of the system are high, which signifies the good anticorrosion property. In Fig. 10(b), the 1 wt% ILGO/epoxy coatings exhibited higher R_pore and R_ct values, measuring 3.41×10⁶ (Ωcm²) and 7.33×10⁶ (Ω cm²), respectively. The EEC results demonstrate that the inclusion of 1 wt% ILGO filler in the epoxy provides effective protection for the carbon steel substrate in the CO₂-NaCl system. Ultimately, the ILGO/epoxy coating acted as a nanosheet barrier, preventing the penetration of corrosive fluid through the coating and effectively separating the carbon steel from the CO₂-NaCl solution. The electrochemical results are consistent with our characterization (FESEM and contact angle analysis) of coating results.

3.5 Corrosion protection mechanism:

The CO₂ molecules react with H₂O in the solution and form ionizable carbonic acid. Although carbonic acid is relatively mild in comparison to other acids, it can induce corrosion depending on the chemical makeup of the material (Rizzo et al. 2020). Tiny gaps are formed inside the pure epoxy coating during the curing process as a result of the shift in internal and external tension. CO₂ molecules, along with carbonic acid (H₂CO₃) molecules, penetrate the surface of the carbon steel substrate due to pressure-driven diffusion. This interaction facilitates the diffusion of corrosive agents through the protective coating, potentially leading to localized corrosion of the substrate (Zhou et al. 2022; Yin et al. 2024b). H₂CO₃ molecules react with the carbon steel substrate due to high polarization, causing carbon steel corrosion.

IL formed a covalent bond with the GO surface, reducing the π–π interactions between the oxygen-containing functional groups in GO, reducing the agglomeration of GO (Yang et al. 2024). ILGO composite exhibits exceptional hydrophobic characteristics, effectively obstructing corrosive substances from reaching the surface of the carbon steel substrate. After IL modification of GO with IL, ILGO composite could be better integrated into the epoxy matrix, thus improving corrosion resistance. Finally, the grafted triethylsulfonium bis-trifluoromethylsulfonyl-imide IL boosts the anticorrosive capabilities by organizing interaction with the carbon steel substrate, which further improves the service life of the composite coatings.

In the recent year researches are focusing on the sustainability and cost-effectiveness synthesis of various ionic liquids (Hussain et al. 2023; Lejeune et al. 2024; Ikeuba et al. 2024). A cost analysis of ILGO/epoxy coatings for commercialization, as well as an evaluation of their mechanical properties, is essential for their application in CCUS industrial settings.

The current study demonstrates an efficient strategy for controlling corrosion, specifically through the use of an anti-corrosive coating, to protect carbon steel in the CCUS technology. This paper describes the preparation of GO using an improved Hummers method, followed by functionalization with an IL. The characterization results, including FESEM, TEM, and XPS, confirmed the successful preparation of the ILGO filler. The ILGO filler is added to the epoxy matrix at two different weight percentages (0.5% and 1%) and coated on the carbon steel with a thickness of 50 ± 3 µm. The results obtained from the FESEM and water contact angle measurements indicated a surface that is free from fractures and pores and has the ability to repel corrosive fluids. Further, electrochemical tests were conducted to analyse the anticorrosion behaviour of the ILGO/epoxy coating in 3.5 wt% NaCl solution. The potentiodynamic polarisation results indicate a significantly high R_p value (2817.05 ± 28.22 Ω cm²) and PE (92.59 ± 0.83%) for the 1 wt% ILGO/epoxy coating. The results from EIS and EEC analysis demonstrate the effective ability of the 1 wt% ILGO/epoxy coating to prevent corrosion in the presence of the CO₂-NaCl system. The results of this article provide valuable insights for choosing an ILGO as an appropriate filler for the epoxy coating in CCUS industrial applications.

Funding:

Not applicable.

Competing Interests:

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Authors Contributions:

Nikhil Rahul Dhongde: Writing – review & editing, Writing –original draft, Visualization, Validation, Methodology, Investigation, Formal analysis, Data curation, Conceptualization, Software. Sayani Adhikari: Data curation, Formal analysis, Software. Prasanna Venkatesh Rajaraman: Supervision, Resources, Project administration, Writing – review & editing.

Acknowledgment

The authors would like to acknowledge the analytical facilities provided by the Central Instruments Facility (CIF) of the Indian Institute of Technology Guwahati, India, Aries Engineer, Maharashtra, India for metal fabrication, Also, acknowledge Meso scale engineering and soft materials lab, Indian Institute of Technology Guwahati, India for providing goniometer to perform contact angle measurements.

Ethical Approval:

Not applicable.

Consent to Participate:

Not applicable.

Consent to Publish:

Not applicable.

Availability of data and materials:

The datasets used and analyzed during the current study are available from the corresponding author on reasonable request.

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Anticorrosion properties of ionic liquid functionalized graphene oxide epoxy composite coating on the carbon steel for CCUS environment

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Abstract

Figures

1. Introduction

2. Experimental work

2.1 Materials

2.2 Synthesis of GO via improved Hummer’s method

2.3 Preparation of ILGO

2.4 ILGO coatings on carbon steel substrate

2.5 Characterization

2.6 Corrosion tests

3. Results and discussion

3.1 Morphology of GO and ILGO:

3.2 X-ray photoelectron spectroscopy (XPS) analysis:

3.3 Characterization of coating:

3.3.1 Morphology analysis by FESEM measurements:

3.3.4 Contact angle measurement:

3.4 Corrosion test of the coating:

3.4.1 Potentiodynamic polarisation test

3.4.2 EIS measurements:

3.5 Corrosion protection mechanism:

4. Conclusion

Declarations

Funding:

Authors Contributions:

Acknowledgment

Availability of data and materials:

References

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