Effect of silane-modified SiO2@Ce3+ nanoparticles on the mechanical property and anti-corrosion for steel of the epoxy coating

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In this work, nano-SiO2 have been used as nanocarriers for loading Ce(III) ions (SiO2@Ce3+). After loading, silane coupling agent has been used to modify these nanocarriers (m-SiO2@Ce3+). Then, these modified nanocarriers were added as green inhibitors into the inner epoxy coating matrix, which was based on the epoxy resin (DER 671X75) and hardener (polyamide Epicure 3125). Morphological study by FE-SEM showed that the spherical nanoparticles (mSiO2@Ce3+) were in size < 100 nm and dispersed rather homogeneously into the polyme matrix.

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Nội dung Text: Effect of silane-modified SiO2@Ce3+ nanoparticles on the mechanical property and anti-corrosion for steel of the epoxy coating

Cite this paper: Vietnam J. Chem., 2023, 61(S3), 109-115 Research Article DOI: 10.1002/vjch.202300060 Effect of silane-modified SiO2@Ce3+ nanoparticles on the mechanical property and anti-corrosion for steel of the epoxy coating Nguyen The Huu1, Dam Thi Tam1,2, Do Truc Vy3, Nguyen Tuan Anh3, Le Trong Lu3, Tran Dai Lam3, Nguyen Thien Vuong3* 1 Faculty of Chemical Technology, Hanoi University of Industry, 296 Cau Dien, Minh Khai, Bac Tu Liem, Hanoi 10000, Viet Nam 2 Hanoi Irradiation Center, Vietnam Atomic Energy Institute, 2PXV+473, Highway 32, Minh Khai, Bac Tu Liem, Hanoi 10000, Viet Nam 3 Institute for Tropical Technology, VAST, 18 Hoang Quoc Viet, Cau Giay, Hanoi 10000, Viet Nam Submitted February 18, 2023; Revised June 20, 2023; Accepted July 20, 2023 Abstract In this work, nano-SiO2 have been used as nanocarriers for loading Ce(III) ions (SiO2@Ce3+). After loading, silane coupling agent has been used to modify these nanocarriers (m-SiO2@Ce3+). Then, these modified nanocarriers were added as green inhibitors into the inner epoxy coating matrix, which was based on the epoxy resin (DER 671X75) and hardener (polyamide Epicure 3125). Morphological study by FE-SEM showed that the spherical nanoparticles (m- SiO2@Ce3+) were in size < 100 nm and dispersed rather homogeneously into the polyme matrix. In addition, the addition of nanocarriers at a concentration of 2.5 wt.% into the epoxy polymer matrix enhanced significantly its mechanical property. Besides, the anticorrosion performance of the epoxy polymer matrix due to the presence of m- SiO2@Ce3+ (at 2.5 wt. %) was proved by EIS analysis and salt spray tests. Keywords. Nano-SiO2 , Ce3+, silane, epoxy, corrosion. 1. INTRODUCTION boosted the adhesion, water adsorption, blistering performance and substrate protection of waterborne Epoxy coating has been widely to protect metals epoxy coatings. againt corrosion, due to good processability, low Recently, researchers are focusing on the smart production cost, high chemical resistance, good organic coatings for anticorrosion with smart dielectric, and strong adhesion to metallic surface.[1- inhibitors- loaded nanocontainers/nanocarriers. This 3] However, the cracking reactions of the epoxy new approach was the combination of nanoparticles coating during the initiation and propagation steps (nanocontainers/nanocarriers) with corrosion limit its application.[4] To overcome this issue, inhibitors. As reported, various inorganic nano-oxides adding nanoparticles as nanofillers into epoxy resin (zirconi dioxide, titania, silica, nanotubes,...) have have been developped.[5-9] As reported, the presence been used as nanocontainer for encapsulation of of nanoparticles in the epoxy matrix enhanced both corrosion inhibitors.[17-19] Among these imorganic its barrier effect for anti-corrosion[9-12] and inhibition nanocontainers, silica nanocontainer is assumably the of trend to blister or delaminate.[13] In this direction, most promising candidate applied in the smart we found the presence of various nanoparticles organic coating due to its dual functions: (i) as an (SiO2, Zn, Fe2O3, clay) in epoxy coating has effective filler at the nanoscale[20,21], and (ii) as an effectively minimized the rate of epoxy-coated steel excellent nano-sized container controllable with being corroded up to 11-910 times in 3 wt. % pH.[18] On this direction, we reported the effect of the NaCl solution.[14] novel Ce-loaded silica nanoparticles (SiO2@Ce3+) in To further improve the corrosion performance of the epoxy nanocomposite coating on the anticorrosion epoxy coating, other approach of using corrosion protection of carbon steel.[22] Our EIS results showed inhibitors as additives has been proposed.[1,15,16] that the presence of SiO2@Ce3+ nanocontainers Galliano and Landolt[1] indicated that modification increased not only the coating resistance but also the by corrosion inhibiting additives significantly polarization resistance of the paint coating. Addition 109 Wiley Online Library © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH
25728288, 2023, S3, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202300060 by Readcube (Labtiva Inc.), Wiley Online Library on [01/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Nguyen Thien Vuong et al. to the enhanced barrier performance, Ce inhibitor agents. Firstly, an amount of 0.5 g dried SiO2@Ce3+ contributed greatly to the anticorrosive activity at the nanoparticles is dispersed in 25 mL of toluene under steel-electrolyte interface. ultrasonication during 30 min. Secondly, a mixture In this study, aim to improve the dispersion of of 0.138 mL GPTS and 0.1 mL TEA is added into SiO2@Ce3+ nanocontainers in the epoxy matrices, the above as-prepared solution, and then stirred we modify SiO2@Ce3+ nanocontainers by silance mechanically at 300 rpm (at 80±5oC) for 1 h. coupling agent (m-SiO2@Ce3+) before adding them Thirdly, the obtained product was centrifuged at to the epoxy coating matrices. 8,000 rpm for 10 min and washed with ethanol. Finally, the solid products are collected and dried at 2. MATERIALS AND METHODS 80oC for 12 h. 2.1. Materials 2.4. Epoxy nanocomposite coating preparation D.E.R.TM 671-X75 Epoxy Resin Solution (Dow) The epoxy/m-SiO2@Ce3+ nanocomposite paint containing nonvolatile content of 74-76 Wt.% and containing 2.5 wt.% m-SiO2@Ce3+ nanoparticles epoxide group of 9-10 wt.% . EPIKURE 3125 was prepared from the epoxy and hardener. The Curing Agent (Hexion) consisting of amine content detailed paint formulation is presented in table 1. equivalent to 330-360 mg KOH/g. Table 1: Formulations of neat epoxy (EP) and epoxy Nano-SiO2 was prepared based on previously nanocomposite (EP-m-SiO2@Ce3+) coatings reported method (Bui, 2020). Ce(NO3)3.6H2O 99.99%, silane coupling agent: (3- EP_m- No Materials EP (g) glycidyloxypropyl)trimethoxysilane (GPTS) ≥ 98% SiO2@Ce3+ (g) are commercial products provided byf Sigma- 1 D.E.R.TM 671-X75 111 111 Aldrich (Singapore) while solvents such as toluene epoxy, g and xylene were supplied by Merck. 2 EPIKURE 3125 48 48 The steel coupons were of steel CT3 (Russian curing agent, g GOST 380-94), 150×100×1 mm, with the chemical 3 Xylene, g 20 20 composition: C 0.14-0.22%, Mn 0.40-0.65%, Si 4 Toluene, g 20 20 0.15-0.30%, Cu 0.25-0.40%, Fe 97.0-98.2%, P ≤ 5 m-SiO2@Ce3+, g 0 3 0.04%, S ≤ 0.05%, S ≤ 0.05%, Cr ≤ 0.3%, Ni ≤ 0.3%, Cu ≤ 0.3%. The preparation is described as follows: The fabricated nanocontainers were ultrasonically 2.2. Fabrication of Ce3+ loaded SiO2 nanoparticles dispersed into solvent mixture for about 100 min using a Telsonic device (25 kHz, Switzerland). After In the first step, about 1.00 gram of silica that, we introduced the epoxy resin D.E.R.TM 671- nanoparticles were unltrasonically dispersed in X75 to the mixture and further sonicated for 100 90 mL of de-ionized water for 15 min. Next, the min. Thereafter, the polyamin EPIKURE 3125 as a aqueous Ce(NO3)3 solution (0.04 M) was poured to hardener was poured to the mixture. Followingly, the silica dispersion and the obtained mixture was the mixture was stirred mechanically at 300 rpm for magnetically stirred for 12 h. Afterwards, the 5 min in order to well-disperse all m-SiO2@Ce3+ mixture was centrifuged at 8,000 rpm for 5 min to nanoparticles into the epoxy matrix. collect the desired particles. To remove The coated substrates could be glass or steel supernatants, the particles were continuously coupons, depending on the aim of further dispersed in fresh distilled water and centrifuged investigation. Particularly, the paint sample on glass until pH of the dispersion reached 7. A white solid was suitable for morphology study whereas, other of SiO2@Ce3+ nanoparticles was dried under tests required it coated on steel plates. For anti- vacuum at 70±5oC for 10 h, then kept in dry storage corrosion studies, the steel coupons with dimensions for further uses. of 150×100×2 mm were used as metal substrate. The coatings were left at normal dry conditions for 7 2.3. Preparation of silane modified Ce3+ days for complete curing. The estimated thickness of (m-SiO2@Ce3+) loaded SiO2 nanoparticles the dried paint films was approximately 20 mm. In order to improve the dispersion of SiO2@Ce3+ 2.5. Characterization nanoparticles into the coating matrix, these nanoparticles are further modified by silane coupling The morphology of the nano SiO2 loading Ce3+ © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 110
25728288, 2023, S3, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202300060 by Readcube (Labtiva Inc.), Wiley Online Library on [01/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Effect of silane-modified SiO2@Ce3+ nanoparticle… inhibitor was observed using a TEM (Transmission After 3-day and 18-day of immersion in the 3% Electron Microscope (JEM 1010, JEOL) and NaCl solution, both epoxy and epoxy nanocomposie SEM/EDX (Scanning Electron Microscopy/Energy coatings were examined by EIS test. The obtained Dispersive X-ray spectroscopy along with EDX. EIS data were fitted by using one simple equivalent (S 4800, Hitachi). Fourier-transform infrared electric circuit (EEC) model (figure 1).[14,22] spectroscopy (FTIR) was provided by NICOLET (IS10, Thermo Fisher Scientific). A MiniTest 600 2.7. Salt spray test (ElektroPhysik, Germany) was used to estimate the average thickness of the sample coatings. The Salt spray test was carried out under JIS H coating adhesion was evaluated by using the cross 8502:1999 standard, using Q-FOG CCT 600 cut test (ISO 2409) with level 0 was the best instrument, with 5% NaCl solution at pH 6.5÷7.2, adhesion and level 5 was the worse adhesion. The injection pressure of 1.0 atm and spray speed 2 ball impact test (model 304, Erichsen) and abrasive mL/h/80 cm2. falling method (ASTM D968 standard) were used to evaluate the impact strength and the falling sand 3. RESULTS AND DISCUSSION abrasion resistance of the coatings, respectively. 3.1. Morphological study of silane modified Ce 2.6. Electrochemical impedance spectroscopy loaded SiO2 (m-SiO2@Ce3+) nanoparticles study of coatings As can be seen from TEM images in figure 2, the EIS were obtained using a Biologic instrument SiO2 nanoparticles with and without inhibitors (VSP-300, France). showed no significant difference in size. Particularly, the average diameters of both nano- SiO2 and SiO2@Ce3+ particles were about 40 nm. However, before loading cerium (figure 2a), the nano SiO2 seemed to be denser. Meanwhile, after cerium loaded, the connection between SiO2 nanoparticles looked more unfasten (figure 2b). This result implies cerium inhibitors had been Figure 1: The fitted equivalent circuit successfully attached on the surface of SiO2 whereas: Rs is the equivalent series resistance, R1 and C1 nanoparticles. symbolize the resistance and the capacitance SEM/EDX study has been used to investigate the characterizing for the epoxy coating, respectively. C2 elemental composition of SiO2@Ce. EDX spectrum stands for the double layer capacitance and R2 quantifies the interfacial charge transfer resistance of the steel- as shown in figure 3 proved the presence of cerium electrolyte contact. The C is fitted as Q, the constant species with the percentage t of ~ 4.7 (by weight of phase element (CPE) of non-ideal capacitor SiO2 nanoparticles). Figure 2: TEM images of: (a) the initial nano-SiO2 particles; and (b) the nano-SiO2 particles with Ce3+ ion attached to their surface (Magnification: × 100,000) To determine the presence of silane groups in spectroscopy was performed (figure 4). As can be the surface of SiO2@Ce nanoparticles, FTIR seen in the figure 4, all of three nanoparticles © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 111
25728288, 2023, S3, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202300060 by Readcube (Labtiva Inc.), Wiley Online Library on [01/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Nguyen Thien Vuong et al. samples (SiO2, SiO2@Ce3+, m-SiO2@Ce3+) had an absorbed on their surface. Interestingly, an absorption peaks at 1106, 805 and 474 cm–1, additional bands of GPTS agent at 2949 and 2866 respectively. These bands characterize for cm-1 were found only on the m-SiO2@Ce3+ sample. oscillations of the Si–O group. Besides, their These bands were the oscillations of alkyl group absorption band at 3446 cm-1 was attributed to the (-CH2/-CH3 asymmetrical and symmetrical OH bond vibration of their H2O molecules. An elongations), which could not find in the FTIR additional band at 1384 cm-1 was observed for spectra of both SiO2 and SiO2 load Ce3+ ions SiO2@Ce3+and m-SiO2@Ce3+ particle samples. This samples. These FTIR data confirmed the successful band could be attributed to the nitrate groups that fabrication of m-SiO2@Ce3+ nanoparticles. Figure 3: EDX pattern of SiO2 carrying Ce nanocontainers Figure 4: FTIR spectra of SiO2, SiO2@Ce3+, m-SiO2@Ce3+ nanoparticles 3.2. Mechanical properties and morphology of kg.cm) and abrasion resistance (from 83 to 130 epoxy nanocomposite coating L/mil.) of the epoxy coating (table 2). In the previous work,[22] with content of SiO2@Ce3+ from Figure 5 shows the cross-sectional FE-SEM images 0-7.5 wt.%, we reported that increasing the content of the epoxy coating reinforced by m-SiO2@Ce3+ of nanoparticles up to 2.5 wt.% led to an increase in nanoparticles (at 2.5 wt.%). Obviously, the abrasion resistance of epoxy coating (from 80 to 120 nanoinhibitors homogeneously dispersed in the L/mil.). But, at the higher contents, the abrasion coating matrix. From the mechanical studies (table resistance decreased. In that work, the nano-SiO2 2), the presence of 2.5 wt.% m-SiO2@Ce3+ has been not modified by silane agent. Thus, the nanoparticles did not change the adhesion of epoxy silane modification of nano-SiO2 might enhance coating on steel substrate. However, the slightly the abrasion resistance of EP-SiO2@Ce3+ incorporation of m-SiO2@Ce3+ nanoparticles coating. Similarity, without silane modification for increased both impact strengh (from 175 to 185 nano-SiO2, the average value of impact strength of © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 112
25728288, 2023, S3, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202300060 by Readcube (Labtiva Inc.), Wiley Online Library on [01/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Effect of silane-modified SiO2@Ce3+ nanoparticle… EP-SiO2@Ce3+ coating was only 185 kg.cm, but it is 195 kg.cm once modified by silane in this study. Figure 5: Cross-sectional FE-SEM images of the epoxy coating loading 2.5 wt.% m-SiO2@Ce3+ 3.3. Effect of m-SiO2@Ce3+ nanoparticles on and steel - electrolyte, at high and low frequencies, eleclectrochemical performance of the epoxy respectively. nanocomposite coatings Nyquist plots of the neat epoxy coated steel and the nanocomposite coated steel after 3 and 18 days of immersion are presented in figures 6 and 7, respectively. Data was best-fitted to the equivalent electric circuit (EEC) model shown in figure 1 and parameters listed in table 3. Table 2: Values obatained from the mechanical studies of EP and EP-m-SiO2@Ce3+ coatings EP-m- No Properties EP SiO2@Ce3+ 1 Ahesion, level 1 1 2 Impact resistance, 175±5 195±5 Figure 6: EIS Nyquist plots of the neat epoxy kg.cm coatings (EP) and m-SiO2@Ce3+ nanoparticles 3 Abrasion resistance, 83±3 130±3 modified coating (EP_m-SiO2@Ce3+) after 3 days of liter/mil immersion in 3% NaCl solution From table 3, we can find an obvious increase of The occurrence probability and condition of the R1 corresponding to the coating electrolyte steel substrate corrosion was monitored by the open resistance of the nanocomposite coating compared to circuit potential (OCP). The OCP values of the neat the neat one. It indicates that the incorporation of epoxy after immersion varied from -590 mV/SCE nanoparticles reduced the coating porosity and then (after 3 days) to -350 mV/SCE (after 18 days). improved the corrosion barrier performance of the Whereas the OCP values of the coating modified by steel substrate.[14,22] This change in coating m-SiO2@Ce3+ nanoinhibitors changed from -280 to - resistance R1 also suggest that the protection from 100 mV. Since Ce3+ is assumed as a cathodic corrosion of the m-SiO2@Ce3+ nanoinhibitors in the inhibitor, the OCP values have tendency to anodic. coating pore network had improved, more This more anodic shift of OCP values is expected to effectively than other reported coating-steel interface increase the impedance on the surface of steel. modification methods. It is believed that the SiO2 As observed in figures 6 and 7, the Nyquist nanoparticles had occupied free spaces in the epoxy diagram which was best-fitted to the obtained EIS coating and served to the interconnection of the data of the neat coating after 18 immersion days matrix, increasing the cross-linking density of the featured clearly two semi circles, representing the cured epoxy and also improving the steel corrosion electrochemical interfaces of coating – electrolyte protection.[14] Regarding the C1 (capacitance of © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 113
25728288, 2023, S3, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202300060 by Readcube (Labtiva Inc.), Wiley Online Library on [01/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Nguyen Thien Vuong et al. epoxy coating), after 18 days of immersion, the C1 A salt spray test using NaCl with a concentration of value of the nanocomposite coating was lower than wt.5% was carried out in a Cyclic Corrosion Tester that of the neat epoxy coating, indicating the lower (Q-FOG CCT 600) based on the standard JIS penetration of electrolyte into the epoxy matrix of H8502. The surface of the as-modified coatings the coating.[14,22] before and after 18 days of salt spray test can be observed in figure 8. The resistance ability to corrosion of the epoxy coating samples was evaluated qualitatively by the appearance of red rust according to the salt spray cycles in the 5% NaCl neutral salt spray test. As seen in Figure 8, after 18 days undergoing the salt spray test, there appeared many spots of red rust on the neat epoxy coating, more than that of nanocomposite coating. Figure 7: EIS Nyquist plots of the neat epoxy (EP) and the m-SiO2@Ce3+ nanoparticles modified coating (EP_m-SiO2@Ce3+) after 18 days being immersed in 3% NaCl solution At low frequencies, as seen in table 3, the modified coating still exhibited the higher value of charge transfer resistances R2 (polarization resistances Rp) of the steel-electrolyte interface. It means that the inhibitors-modified coating had better corrosion protection and slower rate of delamination underneath of coating. Thus, the modification by m- SiO2@Ce3+ nanoparticle had raised the steel-coating interface resistance R2, proving the effective action Figure 8: Photographs of the coated steels before of Ce inhibitor. and after 18 days of salt spray test. Top row: neat epoxy coating. Bottom row: epoxy coating contained 3.3. Salt spray acceleration test 2.5 wt.% m-SiO2@Ce3+ Table 3: Parameters obtained from the best-fitted equivalent circuits for the epoxy- coated steels with surface area of steel electrode of 9 cm2 and d = 3.8 cm after 3 and 18 days immersed in 3% NaCl solution Time of OCP RS R1 C1(F) R2 C2(F) ponding (days) (mV/SCE) (Ω) (Ω) Q1 (F.s(α - 1)) (Ω) Q2 (F.s(α-1)) EP 3 -590 30 24,971 4.66E-8 (α = 0.759) 74,011 3.63E-7 (α = 0.854) 18 -350 30 171,667 1.8E-8 (α = 0.84) 1.06E6 6.1E-6 (α = 0.44) EP-m-SiO2/Ce3+ 3 -280 30 564,811 2.6E-7 (α = 0.6) 1.87E6 3.88E-6 (α = 0.517) 18 -100 30 205,686 2.15E-9 (α = 0.985) 1.4E6 1.61E-6 (α = 0.482) 4. CONCLUSION been attached successfully on the surface of SiO2@Ce3+ nanoparticles (m-SiO2@Ce3+). Data from TEM, EDX and FTIR indicated that FE-SEM images showed that the as-prepared Ce(III) inhibiotor ions have been successfully loaded spherical nanoparticles (m-SiO2@Ce3+) have been on the surface of nano-SiO2 particles (SiO2@Ce3+) at dispersed homogeneously into the epoxy matrix. the content of 4.7% (by weight of nano-SiO2 Data from mechanical tests indicated that adding particles). After loading, silane coupling agent has 2.5wt.% of m-SiO2@Ce3+ nanoinhibitors into the © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 114
25728288, 2023, S3, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202300060 by Readcube (Labtiva Inc.), Wiley Online Library on [01/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Effect of silane-modified SiO2@Ce3+ nanoparticle… epoxy polymer matrix enhanced significantly its 4373. mechanical property. Besides, analysis by EIS and 12. E Huttunen-Saarivirta, GV Vaganov, VE Yudin, J salt spray tests proved that the modification of the Vuorinen. Characterization and corrosion protection epoxy polymer by m-SiO2@Ce3+ also improved properties of epoxy powder coatings containing nanoclay, Prog Org Coat., 2013, 76, 757-767. significantly its anticorrosion performance. 13. N. Wang, K. Cheng, H. Wu, C. Wang, Q. Wang, F. Wang. Effect of nano-sized mesoporous silica MCM- Acknowledgments. 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